dormouse (Member)
04-20-00 20:41
No 108365
      Another simple 2-CB dream -dreamer  Bookmark   


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dreamer
Member   posted 06-03-98 11:11 PM          
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1) 138gr 1,4-Dimethoxybenzene to 170gr 2,5 dimethoxypropriophenone
reference for everyone age 776 of Vogel`s Chemistry or #36 of pihkal (available in internet);
2)170gr 2,5 dimethoxypropriophenone to 2,5 dimethoxypropionic acid
reference: page 818 of Vogel`s chemistry Willgerodt (someone said that you can use n-butyl amine instead of morpholine, but in my dreams there were no problems of getting 500ml of morpholine from sigma for 35 mark, you can get n-butylamine for same price
Yield: in "practical organic chemistry" the yield with p-methoxyphenylacetic acid is ~63% and with propiophenone ~65%

synthesis:
reflux 0.28 mol of 2,5 dimethoxypropionicacid, 0.42 mol sulphur 0.42mol morpholine for 6 hours.
Pour all into water and wait until it crystallises, filter the crystals and let them dry in air. Pour the reaction product into 400ml ethanolic sodium hydroxide solution and reflux for 7hours. Distil off the ethanol,dilute with water 100ml, acidify with HCl (PH <2) and extract 3 times with 75ml ether. Evaporate the solvent and recrystallise from water or diluted ethanol.

3) 2,5 dimethoxypropionic acid to 2,5 dimethoxyphenethylamine: (Schmidt rearrangement Page 665 of vogel's chemistry)
Conversion of a carboxylic acid into an amine by treatment with hydrazoic acid in conc. H2SO4. Hydrazoic acid is generated in situ by adding sodium azide gradually to the carboxylic acid in the presence of concentrated H2SO4 and chloroform.

RCO2H + HN3 --H2SO4--> RNH2 + CO2 + N2

Yield with 3.5 dinitrobenzoic acid to 3,5 dinitroaniline in "vogel's practical organic chemistry": 90%;

proposed synthesis( i don't know if it could work):
Add to 0.24mol of 2,5 dimethoxypropionic acid in 100ml ether and 20ml 99% H2SO4 100ml of chloroform. Raise the TE to 45. Stir rapidly and add 17.5gr (0.27mol) of sodium azide in small portions whilst maintaining the TE at 35-45 C. After all sodium azide has been added raise the TE so that the chloroform refluxes vigorously and maintain this TE and let it reflux for 3 hours. Cool the reaction mixture, dilute with 2l H2O and change the with 25%NaOH PH to >9. Extract with 3*100ml ether. Evaporate off the solvent and distill at full water pressure under vacuum at 195 to get pure water-white 2,5 DMPEA.


If there are other methods to convert 2,5 dimethoxypropionicacid to 2,5 dimethoxyphenethylamine, to 2,5 dimethoxyamphetamine or to 2,5 dimethoxy propanone, PLZ POST.

3) brominate 2,5 dimethoxyphenylethylamine
to 2-CB.
PIHKAL #20 (available in internet)

prices for chemicals:
1kgr 99% sulfur: 23 dmark
500ml morpholine: 35 dmark
1kg Aluminium chloride anhydrous: 48 dmark
500gr 1,4 dimethoxybenzene 98%: 80 dmark
100gr sodium azide: 34 dmark
500gr Propionyl chloride 98%: 27 dmark
100gr Br: 90 dmark
2l anhydrous Ether:50 dmark
or
2.5l DCM: 120 dmark
NaOH, H2O, Hcl,H2SO4,CHLOROFORM ...:<50 dmark
for about 500 dmark you can maybe get 100gr+ 2-CB, which are 3000-5000 doses (20-30mg a dose). If you can sell all this shit for 2 dmark a dose, you will get a lot of money.  ) (if it works!!!)

All chemicals can be ordered from acros,sigma, carlo erba,fisher,..., through drugstores.

Any comments ?


 
dreamer
Member   posted 06-03-98 11:15 PM          
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Sorry for my english
 
dreamer
Member   posted 06-03-98 11:15 PM          
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Sorry for my english
 
Osmium
Member   posted 06-04-98 08:21 AM          
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Does SIGMA really sell their stuff to private persons???
Or did you order through a legitimate company or university?
They belong to SAF (Sigma, Aldrich, Fluka) Chemicals, the toughest bastards to get stuff from. All your prices are in dmark, does that mean you ordered them in Germany?
Did you have to sign an "end user certificate"? (This is necessary for ether in Germany). And what about that propionyl chloride? No problems there??? I also thought morpholine (like piperidine) is quite difficult to get.
BTW, nice synth. There are other organic acid degradation reactions, some of them might be easier, reactions like Curtius, Lossen, Schmidt, Hoffmann etc. Azide is dangerous in big batches.


Osmium
Member   posted 06-04-98 08:21 AM          
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Does SIGMA really sell their stuff to private persons???
Or did you order through a legitimate company or university?
They belong to SAF (Sigma, Aldrich, Fluka) Chemicals, the toughest bastards to get stuff from. All your prices are in dmark, does that mean you ordered them in Germany?
Did you have to sign an "end user certificate"? (This is necessary for ether in Germany). And what about that propionyl chloride? No problems there??? I also thought morpholine (like piperidine) is quite difficult to get.
BTW, nice synth. There are other organic acid degradation reactions, some of them might be easier, reactions like Curtius, Lossen, Schmidt, Hoffmann etc. Azide is dangerous in big batches.


quirks
Member   posted 06-04-98 08:36 AM          
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I've been trying to find a north american reseller of sigma who sells to individuals FOREVER! I want that ecstasy testing liqued, and everytime I call someone and say "amphetamine" over hte phone it's CLICK! self rightoues bastards...
Anyways, if someone knows the name of a sigma reseller who sells to individuals would you please email me - quirks@nym.lycaeum.org - I'm not going to order chemicals, cause there are multiple local sources for that


quirks
Member   posted 06-04-98 08:36 AM          
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I've been trying to find a north american reseller of sigma who sells to individuals FOREVER! I want that ecstasy testing liqued, and everytime I call someone and say "amphetamine" over hte phone it's CLICK! self rightoues bastards...
Anyways, if someone knows the name of a sigma reseller who sells to individuals would you please email me - quirks@nym.lycaeum.org - I'm not going to order chemicals, cause there are multiple local sources for that


nomadic
unregistered   posted 06-04-98 10:09 AM           
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Are you talking about Marquis (?) kits???...
 
nomadic
unregistered   posted 06-04-98 10:09 AM           
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Are you talking about Marquis (?) kits???...
 
quirks
Member   posted 06-04-98 11:41 AM          
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Yea, the marquis kits. The green party sells them in the UK buy they are expensive and they are buying them from Sigma as well, and there's a haz mat charge for overseas shipping (mucho $$). Cmon people! Give me a sigma supplier!
 
quirks
Member   posted 06-04-98 11:41 AM          
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Yea, the marquis kits. The green party sells them in the UK buy they are expensive and they are buying them from Sigma as well, and there's a haz mat charge for overseas shipping (mucho $$). Cmon people! Give me a sigma supplier!
 
dreamer
Member   posted 06-04-98 12:59 PM          
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I can give only info on resellers of italy and austria. try looking on internet and you can find a few resellers of carlo erba, fluka, sigma, acros in italy, which accept orders by email from private persons  )
 
dreamer
Member   posted 06-04-98 12:59 PM          
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I can give only info on resellers of italy and austria. try looking on internet and you can find a few resellers of carlo erba, fluka, sigma, acros in italy, which accept orders by email from private persons  )
 
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