Rhodium (Chief Bee)
10-25-02 09:04
No 372464
      J-CLANDEST-LAB-INVEST-CHEM-ASS  Bookmark   

ChemisTris found this list of abstracts for us - can anybody of you get this publication?

TI:  Identification of the Potassium Salt of Gamma-Hydroxybutyrate (GHB-K+)
AU:  Walker-L
AD:  California Department of Justice; Freedom Laboratory; 440 Airport Boulevard; Building A; Watsonville; CA 95076; USA
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (1); January; P17-21
PY:  1999
AB:  During the analysis of chemicals seized from a suspected gamma-hydroxybutyrate (GHB) laboratory, it was found that  the dried sample did not have the characteristics associated with the sodium salt of GHB. Based on the suspect's  confession, the sample was suspected of being the potassium salt of GHB, and it was speculated that the infrared (IR)  spectrum and consistency of the drug may differ from that of the sodium salt of GHB. A method is presented for the  determination of the potassium salt of GHB in unknown samples. This method involves initial colour screening tests  and confirmation by gas chromatographic-mass spectrometric (GC-MS) analysis and FTIR analysis.

TI:  Possible New Pseudoephedrine Source Discovered
AU:  Willers-Russo-L-J
AD:  Los Angeles County Sheriff's Department; Scientific Services Bureau; 2020 West Beverly Boulevard; Los Angeles; CA  90057; USA
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 2000; V10 (2); April; P14-17
PY:  2000
AB:  This paper reports a possible new source of pseudoephedrine which was discovered during the investigation of a  suspected clandestine laboratory. The source was an equine product which was marketed as an antihistamine and  decongestant under the name "Tri-Hist Granules." The label stated that this preparation contained 600 mg  pseudoephedrine hydrochloride and 600 mg pyrilamine maleate. In order to determine whether this preparation could  serve as a source of pseudoephedrine, four extraction techniques were used to extract pseudoephedrine from four  one-ounce samples. The extraction methods only succeeded in extracting around one-third of the available  pseudoephedrine at best, therefore the low yield and high extraction effort may not be worth the trouble to illicit  manufacturers.

TI:  Analogues of GHB. Part 1: Theoretical Perspective
AU:  Morris-J-A
AD:  MO State Highway Patrol Crime Laboratory; Troop D Satellite Laboratory; 700 E. Cherry; Springfield; MO 65806; USA
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 2000; V10 (2); April; P18-20
PY:  2000
AB:  In recent years the United States has seen the rise of GHB (gamma-hydroxybutyrate) as a drug of abuse. What can now  be expected is the introduction of analogues of GHB into the circles of GHB abusers. This paper provides a brief  overview of the history of GHB and discusses a number of potential GHB analogues which may be the drugs of abuse of  the future.

TI:  Reaction Byproducts of Common Cold Tablet Ingredients Via Hydriodic Acid/Red Phosphorus
AU:  Oulton-S-R; Skinner-H-F
AD:  Drug Enforcement Administration; Southwest Laboratory; National City; CA 91950; USA
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (4); October; P21-35
PY:  1999
AB:  With restrictions limiting the availability of pure ephedrine or pseudoephedrine, those operating clandestine  methylamphetamine (MA) laboratories in the United States are increasingly using common cold tablets which contain  ephedrine or pseudoephedrine and other ingredients such as paracetamol, chlorpheniramine, dextromethorphan,  diphenhydramine, doxylamine, guaifenesin, and triplodine. Bearing in mind that the synthesis route of choice in these  laboratories is the reduction of ephedrine or pseudoephedrine with hydriodic acid (HI) and red phosphorus (Red P),  each of the common ingredients found in common cold tablets was reacted with HI and Red P to determine if byproducts  were formed which could enable chemists to determine the source of the ephedrine or pseudoephedrine precursors in the  illicit manufacture of methylamphetamine.

TI:  The Synthesis of 2,5-Dimethoxy-4-ethylthiophenethylamine (2C-T-2). A Case Report
AU:  Poortman-Van-Der-Meer-A-J
AD:  Forensic Science Laboratory; Ministry of Justice; Volmerlaan 17; 2288 GD Rijswijk; The Netherlands
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (4); October; P17-20
PY:  1999
AB:  The chemical analysis of several liquids and solids seized from a clandestine laboratory revealed the presence of  intermediates and the final product of the synthesis of 2,5-dimethoxy-4-ethylthiophenethylamine (2C-T-2). The  synthesis of this compound has been described by Shulgin and Shulgin, and is shown in this paper. The chemicals  submitted to the laboratory and the results of the analysis agreed with the method described by Shulgin and Shulgin.  This paper presents the results of the analysis carried out in this case.

TI:  Clandestine Manufacture of Tetrahydrocannabinol Precursors
AU:  Mitchell-W-J; Pearson-J-R; White-M-J
AD:  Victoria Forensic Science Centre; Victoria Police; Forensic Drive; Victoria 3085; Australia
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (2-3); P29-38
PY:  1999
AB:  During the investigation of a suspected clandestine laboratory, large quantities of chemical glassware and over one  hundred unexplained chemicals were discovered. Among the chemicals were two precursors used in the manufacture of  tetrahydrocannabinol (THC), namely, citral and boron trifluoride, and an unknown liquid. Following chemical analysis,  the liquid was found to contain, among other things, olivetol. Of the other components, two were identified as  dimethylolivetol and 1-(3,5-dimethyoxyphenyl)-1-pentanone. The results indicated the possibility of this liquid being  a crude reaction material from the conversion of the ketone to dimethylolivetol and then to olivetol. High purity THC may be manufactured using citral, olivetol and boron trifluoride, despite the difficulties involved  in obtaining the equipment and chemicals.

TI:  Impurities in Methamphetamine Manufactured from Over-The-Counter Pseudoephedrine Tablet Preparations
AU:  Melgoza-L
AD:  CA Dept. of Justice; Riverside Laboratory; 1500 Castellano Road; Riverside; CA 92509; USA
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (2-3); P21-28
PY:  1999
AB:  In Southern California, the most popular method for the illicit manufacture of methamphetamine is the reduction of  ephedrine by hydriodic acid and red phosphorus, but the ephedrine precursor has been appearing les often.  Investigation of clandestine laboratory sites has revealed the presence of empty pseudoephedrine product packaging  and tablets of over-the-counter pseudoephedrine preparations. Some of these products contain only pseudoephedrine,  but others may contain a number of medically active constituents. Such constituents have been identified as  impurities in samples of methamphetamine which have been submitted to the laboratory for analysis. This paper studies  the main impurities found in methamphetamine manufactured using a number of over-the-counter pseudoephedrine  preparations by the hydriodic acid and red phosphorus reduction method.

TI:  DEA Publishes Special Surveillance List for Clandestine Laboratory Supplies and Chemicals
AU:  Marshall-D-R
AD:  None
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (2-3); P11-13
PY:  1999
AB:  On the 3rd of October, 1996, the Comprehensive Methamphetamine Control Act was signed into United States law. This  Act makes it illegal for anyone to distribute a laboratory supply to anyone who uses or attempts to use, that supply  for the manufacture of illicit substances or listed chemicals, with reckless disregard for the illegal uses to which  such supplies will be put. Individuals found to be in violation of this Act are subject to a fine of up to $25,000,  whilst businesses which violate the Act are subject to a fine of up to $250,000. The definition of a "laboratory  supply" in this cases is "a listed chemical or any chemical, substance, or item on a special surveillance list  published by the Attorney General, which contains chemicals, products, materials, or equipment used in the  manufacture of controlled substances and listed chemicals." This paper lists the "laboratory supplies" constituting  the Special Surveillance List.

TI:  Laboratory Seizures
AU:  Doerr-J; Schreiber-L; Laing-R; Block-R; Sorokin-V; Warburton-K; Skinner-H; Chandley-B; Ginn-B
AD:  None
SO:  () J-CLANDEST-LAB-INVEST-CHEM-ASS; 1999; V9 (2-3); P7-10
PY:  1999
AB:  This paper describes a number of seizures from clandestine laboratories. Particular attention is paid to the range of  precursor chemicals found and the methods used in the illicit manufacture of methylamphetamine,  methylenedioxymethamphetamine (MDMA) and 2C-B.

TI:  New Synthetic Drugs in the European Union
AU:  King-L-A; Poortman-Van-Der-Meer-A
AD:  Drugs Intelligence Unit; Forensic Science Service; 109 Lambeth Road; London; SE1 7LP; UK
SO:  J-CLANDEST-LAB-INVEST-CHEM-ASS; 1998; V8 (3); July; P13-14
PY:  1998
AB:  A so-called 'Joint Action' initiative for synthetic drugs was set up by EU member countries in 1997 , dealing with synthetic drugs not under international control. Most of the new drugs are substituted phenethylamines. These new synthetic drugs, which have been reported in at least one EU member country, are listed.

TI:  Designer Drugs Related to Amphetamine (1990-1996)
AU:  King-L-A
AD:  Drugs Intelligence Laboratory; The Forensic Science Service; Aldermaston; Berkshire; RG7 4PN; UK
SO:  J-CLANDEST-LAB-INVEST-CHEM-ASS; 1996; V6 (3); July; P15-16
PY:  1996
AB:  The aim of this short review is to consider those analogues of amphetamine found in street samples or recovered from clandestine laboratories in various countries over the past 6 years, and are for the most part not widely controlled by law. Details are given of 21 substances reported together with notes on the circumstances and likely precursors. In all cases, the named substance was either being synthesised or was the primary drug in illicit powders or tablets in such amounts that it was thought unlikely to have been merely a synthetic impurity. In addition, the synthesis of 3-methoxy-4,5-methylene-dioxyamphetamine (MMDA) using myristicin extracted from nutmeg was being attempted at a clandestine laboratory in the U.K. in 1994. Reports from Germany have described abortive attempts to manufacture 2,5-dimethoxy-4-(n)-propylthiophenethylamine (2C-T-7), other 4-alkylthiophenethylamines, and 4-allyloxy-3,5-dimethoxyphenethylamine.

TI:  Unusual Defense to Charge of MDMA Manufacture
AU:  King-L-A; Clarke-K; Scott-R-J
AD:  Drugs Intelligence Lab, FSS, Aldermaston, Reading, Berks, RG7 4PN, UK
SO:  J-CLANDEST-LAB-INVEST-CHEM-ASS; 1995; V5(3); July; P6
PY:  1995
AB:  In late 1993 in Takeley, Essex, UK, a laboratory on a light industrial estate was raided by police officers. Amongst the significant findings were sixteen 2L conical flasks with an odour of methylamine each containing a yellow liquid above a grey sludge. Subsequent analysis showed that the flasks contained, in total, an estimated 1.3kg of 3,4-methylenedioxymethylamphetamine (MDMA). Numerous containers of acids, alkalis and solvents were found as well as hydrogen peroxide, mercuric chloride, aluminium foil, formic acid, and methylamine. Traces of safrole and isosafrole in an acetone solution were also detected. Documents recovered from the scene included articles on isosafrole and photocopies of those pages in PIHKAL [1] which relate to the synthesis of MDMA by the aluminium foil route from 3,4-methylenedioxyphenyl- 2-propanone (piperonylmethylketone, PMK).

TI:  Clandestine Laboratories in the UK
AU:  King-L-A; Glasgow-S
AD:  DIL, FSS, Aldermaston, Reading, Berks, RG7 4PN, UK
SO:  J-CLANDEST-LAB-INVEST-CHEM-ASS; 1994; V4(1); January; P19-20
PY:  1994
AB:  This article describes the current illicit laboratory situation in the UK. The term `illicit' is used in a restrictive sense to describe the production of controlled drugs, but clandestine laboratories producing non-controlled drugs (e.g. steroids and othe counterfeit medicines) are occasionally seen. In the UK, the unauthorised production of controlled drugs is an offence under the Misuse of Drugs Act 1971. In this legislation, `production' covers both cultivation as well as manufacture by synthesis. Only synthetic laboratories will be considered here, but laboratories engaged in growing cannabis plants by hydroponic/artificial light methods are becoming increasingly common.
 
 
 
 
    Bubbleplate
(Hive Bee)
10-26-02 04:30
No 372730
      Whats With The Freon????  Bookmark   

Is Freon used by Euro chemists or what's up with that:

The MCA provides for a civil penalty of not more than $250,000 for the distribution by a business of a laboratory supply to a person who uses, or attempts to use, that laboratory supply to manufacture a controlled substance or a listed chemical, if that distribution was made with ``reckless disregard'' for the illegal uses to which such a laboratory supply would be put. 21 U.S.C. 842(a)(11), 842(c)(2)(C). Individuals who violate 21 U.S.C. 84(a)(11) are subject to a civil penalty of not more than $25,000. 21 U.S.C 842(c)(1)(A). For purposes of this provision, the term ``distribution'' includes the exportation of a laboratory supply.
The MCA further states that, for purposes of 21 U.S.C. 842(a)(11), there is a ``rebuttable presumption of reckless disregard at trial if the Attorney General notifies a firm in writing that a laboratory supply sold by the firm, or any other person or firm, has been used by a customer of the notified firm, or distributed further by that customer, for the unlawful production of controlled substances or listed chemicals a firm distributes and 2 weeks or more after the notification the notified firm distributes a laboratory supply to the customer.''
The CSA contains other sections relating to the illegal manufacture of controlled substances. Section 841(d)(2) of Title 21 provides that any person who knowingly or intentionally distributes a listed chemical knowing, or having reasonable cause to believe, that it will be used in the illegal manufacture of a controlled substance, is subject to criminal prosecution. Section 843(a)(7) of Title 21 provides that any person who knowingly or intentionally distributes any chemical, product, equipment or material which may be used to manufacture a controlled substance or listed chemical, knowing, intending, or having reasonable cause to believe, that it will be used to mauufacture a controlled substance or listed chemical, is subject to criminal prosecution.
In developing the Special Surveillance List, the DEA consulted with both DEA and State/Local law enforcement and forensic laboratory authorities. The DEA examined clandestine laboratory seizure reports for information regarding: (1) Illicit drug production methods; (2) chemicals actually used in clandestine production of controlled substances and listed chemicals; and (3) the role and importance of chemicals used in the syntheses. In addition, the DEA considered the legitimate uses and market for these chemicals.
The Special Surveillance List focuses on chemicals used in the domestic production of controlled substances and listed chemicals. Therefore the list includes those chemicals used not only in the production of methamphetamine, but also of other controlled substances such as PCP, LSD, methcathinone and amphetamine. The list does not focus on chemicals used in the production of heroin or cocaine since these drugs are seldom produced domestically. However, the Special
Surveillance List includes all listed chemicals as specified in 21 CFR 1310.02 (a) or (b). The phrase ``all listed chemicals'' includes all chemical mixtures and all over-the-counter (OTC) pharmaceutical products and dietary supplements which contain a listed chemical, regardless of their dosage form or packaging and regardless of whether the chemical mixture, drug product or dietary supplement is exempt from regulatory controls.
The following is the Special Surveillance List for laboratory supplies used in the manufacture of controlled substances and listed chemicals:

Special Surveillance List Published Pursuant to Title 21, United States Code, Section 842(a)(11)
Chemicals
All listed chemicals as specified in 21 CFR 1310.02 (a) or (b). This includes all chemical mixtures and all over-the-counter (OTC) products and dietary supplements which contain a listed chemical, regardless of their dosage form or packaging and regardless of whether the chemical mixture, drug product or dietary supplement is exempt from regulatory controls.
Ammonia Gas
Ammonium Formate
Bromobenzene
1,1-Carbonyldiimidazole
Cyclohexanone
1,1-Dichloro-1-fluoroethane (e.g. Freon 141B)
Diethylamine and its salts
2,5-Dimethoxyphenethylamine and its salts
Formamide
Formic Acid
Hypophosphorous Acid
Lithium Metal
Lithium Aluminum Hydride
Magnesium Metal (Turnings)
Mercuric Chloride
N-Methylformamide
Organomagnesium Halides (Grignard Reagents) (e.g. ethylmagnesium bromide and phenylmagnesium bromide)
Phenylethanolamine and its salts
Phosphorus Pentachloride
Potassium Dichromate
Pyridine and its salts
Red Phosphorus
Sodium Dichromate
Sodium Metal
Thionyl Chloride
ortho-Toluidine
Trichloromonofluoromethane (e.g. Freon-11, Carrene-2)
Trichlorotrifluoroethane (e.g. Freon 113)
Equipment
Hydrogenators
Tableting Machines
Encapsulating Machines
22 Liter Heating Mantels
Individuals and firms which distribute listed chemicals and chemicals, products, materials, or equipment on the above list, are hereby officially notified that these materials may be used in the illicit production of certain controlled substances or listed chemicals.

 
 
 
 
    Rhodium
(Chief Bee)
10-26-02 05:39
No 372747
      Euro chemists never use freon - I think I haven't ...  Bookmark   

Euro chemists never use freon - I think I haven't seen anything here using CFC's since the 1980's. But for examples of irresponsible use of freon in the US just check the stimulants forum - some use it because they don't want to heat a solution to boil off the solvent, and thus extract with a freon with a bp below ambient temp...
 
 
 
 
    Aurelius
(Hive Bee)
10-26-02 07:27
No 372776
      Freon  Bookmark   

always wondered why those were on that list.  guess know it's known. 
 
 
 
 
    El_Zorro
(Hive Bee)
10-27-02 02:28
No 373033
      I remember when I was younger I used to shoot old ...
(Rated as: dangerous)
 Bookmark   

I remember when I was younger I used to shoot old air conditioners with a .22 to see the freon spray out.

Who is that masked man?
 
 
 
 
    GC_MS
(Hive Bee)
11-02-02 16:23
No 375729
      J-CLANDEST-LAB-INVEST-CHEM-ASS  Bookmark   

Maybe we should start our own journal... J Clandest Lab Owners Chem Ass... Any bee with too much time? laugh

Ave Hive, synthetisandi te salutant!
 
 
 
 
    Rhodium
(Chief Bee)
11-02-02 19:17
No 375757
      Journal of Clandestine Chemistry  Bookmark   

In 1998 I tried to start an online journal called "Journal of Clandestine Chemistry", but in three months I only got two submissions, one was the incredible PCP synthesis review by Beagle, and the other one was Ritter's Nitromethane/MDP2P Al/Hg reductive amination, which later evolved into the "MM Al/Hg".

Great submissions, but I realized that unless I did everything myself, there wouldn't be enough material to even make it a quarterly journal. I still have the HTML for the draft journal homepage though.
 
 
 
 
    GC_MS
(Hive Bee)
11-02-02 19:47
No 375773
      2002  Bookmark   

Well, 1998 is about four years ago. You might want to call for another try? wink Obviously, nobody is looking your direction to organize this journal from the beginning to the end. We all know you have your hands full already. Candidates?
The mentioned submissions are full syntheses. You can use several categories: novel routes, method improvement, theoretical section, new laws, comments etc etc etc etc etc. You could require submission in PDF, so one should only merge the PDFs to a final journal. Only my thoughts... But if you see that the CLIC can edit a journal every month, we should be able to do at least the same cool

Ave Hive, synthetisandi te salutant!
 
 
 
 
    Rhodium
(Chief Bee)
11-02-02 20:42
No 375790
      J. Cland. Chem.  Bookmark   

In the last call, I DID request book reviews, news, laws, communications etc.

See ../rhodium/archive/jcc/ for how the silly draft looked like. The HTML is a little off, as the 1999 version of Netscape HTML is not what current browsers are like...
 
 
 
 
    yellium
(I'm Yust a Typo)
11-02-02 20:58
No 375793
      You could also see it as a 'best of' of your ...  Bookmark   

You could also see it as a 'best of' of your website :-).
 

When all you've got is a nailgun, every problem looks like a messiah...
 
 
 
 
    GC_MS
(Hive Bee)
11-02-02 21:46
No 375802
      shame  Bookmark   

Shame, really looks good crazy. I'd prolly put a list with PDFs online; would have been easier (I think).
Getting your hands on the journal mentioned in the thread title is near to impossible. Unless... there is a bee present who works in a DEA office and is directly involved in forensic chemistry research [cough]. Anyone [cough] [cough]? If you belong to this category, you know you could do us a huge favour smile.

Ave Hive, synthetisandi te salutant!
 
 
 
 
    randolph_carter
(Hive Bee / Eraser)
11-04-02 23:07
No 376450
      did i hear JCC again????  Bookmark   

well howdee.....

I hear the sounds of jcc again!!!!
is it echoes......echoes......echoes or just memorex....???
anyhoo if'n yer needin submissions i could upload me "Adventures In Asarone Land" novella for publication....
also "Industrial Scale Techniques For MA And Other Psych Amphets Via Tube And Bomb" i remember well the bandying about of JCC....and thought it would be a hoot!!!

ya letz do itz!!!!!

jus a ravin inta da birdseye on a late afternoon....

"remember little ones, love is real,not fade away, so pass some ammo on today......"
 
 
 
 
    Rhodium
(Chief Bee)
11-04-02 23:23
No 376457
      Randolph Carter  Bookmark   

You know my email. Send in your submissions immediately. What's your response to Post 369697 (Ritter: "Warning on RC's Leukart!", Methods Discourse) btw?
 
 
 
 
    randolph_carter
(Hive Bee / Eraser)
11-27-02 17:56
No 383918
      reply to alledged "low" leukart yields.....  Bookmark   

I have been watching the discussions for some time and I have exception with ritter's allegation that the leukart is low yielding....
actually when applied to unhintered p2p's ie straight p2p and n-methylformamide it approaches 100%...
note i stated "approaches" not =100%....
it is more of an art than a technique tho....
the skill and attention to ALL details of the worker bee is more important than any other single variable....

as to other leukart raves on the hivage that have more than 30% yields....

see these linkages....

Post 302161 (Antoncho: "Leuckart with 92%+ overall yield", Methods Discourse)
Post 61613 (psyloxy: "Re: Leukard scaleable ?", Methods Discourse)
Post 27089 (Chopper_: "Re: Ducks need help with Leukart", Methods Discourse)
Post 240004 (PolytheneSam: "Re: Benzedrine method", Stimulants)
lizards KNOW that high yields are in fact doable not just possible!!!!

jus my lil 64,362 cents worth in the am....




"remember little ones, love is real,not fade away, so pass some ammo on today......"
 
 
 
 
    terbium
(Old P2P Cook)
11-27-02 19:33
No 383944
      BS  Bookmark   

actually when applied to unhintered p2p's ie straight p2p and n-methylformamide it approaches 100%...
That is certainly not my experience. I stand by the 30% value but if you know the secret of near 100% yields then tell us.

it is more of an art than a technique tho....
Oh, I see, it is something that can not be explained with words. Do you also generate all of your electricity via cold fusion?

see these linkages....

Antoncho: "Leuckart with 92%+ overall yield" (Methods Discourse)
psyloxy: "Re: Leukard scaleable ?" (Methods Discourse)
Chopper_: "Re: Ducks need help with Leukart" (Methods Discourse)
PolytheneSam: "Re: Benzedrine method" (Stimulants)

These links are all for the Leuckart done with formamide not n-methylformamide.





Baseline Does Not Exist.
 
 
 
 
    flipper
(Hive Bee)
11-28-02 22:07
No 384365
      cahfigdagfgzhhjxc  Bookmark   


Antoncho: "Leuckart with 92%+ overall yield" (Methods Discourse)




This one is with (Methyl)Ammonium Formate, and hydrolysis with NaOH. Very easy method laugh

 
 
 
 
    Rhodium
(Chief Bee)
11-28-02 22:41
No 384378
      Has it been reproduced outside Russia yet?  Bookmark   

Has it been reproduced outside Russia yet?
 
 
 
 
    terbium
(Old P2P Cook)
11-28-02 22:46
No 384380
      Not that I can see.  Bookmark   


--------------------------------------------------------------------------------

Antoncho: "Leuckart with 92%+ overall yield" (Methods Discourse)




--------------------------------------------------------------------------------


This one is with (Methyl)Ammonium Formate, and hydrolysis with NaOH. Very easy method 

Where does this thread give procedure or yield using n-methylammonium formate?


Baseline Does Not Exist.
 
 
 
 
    Rhodium
(Chief Bee)
11-29-02 02:37
No 384447
      actually, there is something...  Bookmark   

In the end of the first section, it says "Interestingly, if formamide or N-subst'd formamide is used instead of ammonium formate, the yield drops to <70% - DMF giving the ugliest yield of all." in regards to the formation of the formylamine. The document does not detail the hydrolysis of that to the N-Methyl amine though.

Everything about the synthesis sounds good, but its vagueness reminds me of Berichte articles from the early 1900's.
 
 
 
 
    flipper
(Hive Bee)
11-29-02 17:12
No 384603
      oops  Bookmark   


Where does this thread give procedure or yield using n-methylammonium formate?




Stupid chemical names.

Methylammonium formate for MDMA and Ammonium Formate for MDA.

 
 
 
 
    Rhodium
(Chief Bee)
11-29-02 17:56
No 384610
      (MD)MA without methylamine  Bookmark   

Then of course is the possibility of making N-formyl-(MD)amphetamine using ammonium formate/(MD)P2P, and then reduce the amide to (MD)MA with NaBH4 plus a metal salt (ZrCl4, CoCl2, NiCl2, LiCl etc).

That way you can arrive at (MD)MA from (MD)P2P without the need for any methylamine, and the yields should be similar to that from the Al/Hg reductive amination.
 
 
 
 
    flipper
(Hive Bee)
01-12-03 21:53
No 397610
      so  Bookmark   

When you use methylamonium formate and follow the procedure as in Antoncho's post you will not have a high yield of MDMA?????. Why not?
 
 
 
 
    PolytheneSam
(Master Searcher)
01-12-03 22:21
No 397621
      What happened to this?  Bookmark   

What happened to this?
 ../rhodium/archive/leuckart.pdf

Go to http://briefcase.yahoo.com , log in as everybee2, password = allbees and then go to
http://briefcase.yahoo.com/apis_mellifica2002
Look in the Leuckart Reaction folder. 
You need a TIFF browser plug in to view, ie. from http://www.alternatiff.com

http://www.geocities.com/dritte123/PSPF.html
The hardest thing to explain is the obvious
 
 
 
 
    Organikum
(Hive Addict)
01-12-03 23:54
No 397643
      this was what happened:  Bookmark   

../rhodium/pdf /leuckart.pdf

Rhodium reorganized his page a some weeks ago.

ORG

now or never
 
 
 
 
    flipper
(Hive Bee)
01-15-03 12:19
No 398392
      leukart  Bookmark   


Leuckart Reaction
Methylamine is substituted in the Leuckart reaction for MDA to produce MDMA[57]. This is elaborated below. Uncle Fester[58] describes generating high purity N-methyl formamide[59] and then carefully reacting this with phenylacetone for highest yield of methamphetamine. Substituting piperonylacetone for phenylacetone would give MDMA. Fester gives long "idiot proof" directions so I refer you to his book for his directions.

To a three-necked flask equipped with a dropping funnel, thermometer (into the reaction mixture), and down directed condenser (simple distillation apparatus) is added with 133g (1.72 moles) of 40% methylamine solution and 88g (1.72 moles) of 90% formic acid. The temperature is raised to 160C by distilling out water, and 59.4 grams (0.334 moles) of piperonylacetone is added at one time. The following apparatus can be substituted for a three-neck flask and the piperonylacetone added by momentarily replacing the thermometer with a funnel. The mixture is maintained at 160-170C for 7 hours and any ketone which distills over is periodically returned to the flask. The formyl derivative is hydrolyzed in the reaction mixture by refluxing for eight hours with 120 ml of concentrated HCl (145ml 31.5% muriatic acid). The mixture is diluted with 200 ml of water and extracted with benzene (or ether etc.) to remove water insoluble material. The aqueous solution is treated with a little charcoal, Norit (or filtered through activated charcoal from pet stores). The solution is made alkaline with ammonia (or alternatively 25% NaOH) and the oil thus produced is extracted with benzene (or ether etc.). The benzene is washed three times with water and dried with sodium sulfate or other drying agent. A stream of HCl gas is fed through the solution until no more precipitate is formed. The precipitate is filtered out and allowed to dry.

40% methylamine is the commonly available form along with methylamine hydrochloride. Basifying 116g of methylamine hydrochloride with 68.5g of NaOH in 80 ml of water will approximate the 40% solution called for. Slowly add the methylamine hydrochloride to the NaOH solution after it cools. Keep the solution cool to maximize the solubility of the methylamine.

Substituting ethylamine will give Eve.




If it give a high yield of Meth wouldn't it also give a high yield of MDMA????????

 
 
 
 
    GC_MS
(Hive Bee)
01-15-03 14:41
No 398407
      *  Bookmark   


If it give a high yield of Meth wouldn't it also give a high yield of MDMA????????




No, not necessarely. MDMA is Ph ring substituted.


Ave Hive, synthetisandi te salutant!