Glacial_Refluxer (Stranger)
05-22-03 17:37
No 434831
      Myristicin > MMDA advice needed  Bookmark   

Swim is vary interested in trying this synth
../rhodium/chemistry /mmda.html

Can swim use 30% ammonium hydroxide with extended time to
aminate or is anhydrous ammonia required?

http://www.redcoat.net/pics/arguing.jpg
 
 
 
 
    moo
(Hive Bee)
05-22-03 18:13
No 434841
      You need to study chemistry.  Bookmark   

You need to study chemistry. Don't forget to read PIHKAL either. Screw-ups can cost you a lot more than money and you are going to screw up if you don't know the basics. No offense, because that's the way it is.

fear fear hate hate
 
 
 
 
    Glacial_Refluxer
(Newbee)
05-22-03 18:35
No 434845
      Thanks but.....  Bookmark   

Your post did not help at all. PIHKAL synths are a bit more
than swim wants to deal with, to many chems involved.

So can this amination take place with h2o present?

http://www.redcoat.net/pics/arguing.jpg
 
 
 
 
    Antibody2
(Hive Addict)
05-22-03 19:09
No 434852
      Bubble thru 35mL anhydr.  Bookmark   

Bubble thru 35mL anhydr. MeOH in an ice/salt bath

anhydr.=anhydrous=no water
you don't want water
 
 
 
 
    Rhodium
(Chief Bee)
05-22-03 20:07
No 434872
      My advice: Use another method  Bookmark   

I thought I had removed that document already, due to the procedure very likely being at least partly bull. I haven't heard of anyone ever successfully repeating that experiment by IudexK, while I get tons of PM's from people asking me to tell them what they did wrong when trying to get any product from it.
 
 
 
 
    hypo
(Hive Addict)
05-23-03 00:26
No 434912
      which stepd doesn't work?  Bookmark   

a friend of a friend ended up with nearly only polimerised crap
after doing an performic on iso-myristicin (pump probably too
weak), so he is quite interested in this method.

do you know which step is bogus?

what i'm thinking about is reacting the (fractionated) myristicin
with HI in an organic solvent (for example AcOH or DCM?), then
recrystallise it.

the amination would be done pretty much IudexK style (with
magnetic stirring). i figure the big problem here is the
production of secondary and higher amines. but phtalimide and
hydrazine are not available. frown

is that sound, or should my foaf not waste precursors?
 
 
 
 
    Antibody2
(Hive Addict)
05-23-03 05:39
No 434951
      Hypo-i expect if there were problems it wasn't  Bookmark   

Hypo-i expect if there were problems it wasn't that reaction(modifiied performic), much more likely too hot a distillation, IMHO.

ended up with nearly only polimerised crap
after doing an performic on iso-myristicin
my sister has seen sucessful performic oxidations of both iso-myristicin and iso-apiole(dill and parsley). In yields that are comparable to what is acheived using safrole.

She said if she had it to do again she would do it the samesmile
 
 
 
 
    hypo
(Hive Addict)
05-23-03 06:18
No 434957
      yes,  Bookmark   

i know. that's why i said i think the pump is too weak. the non polimerised
fraction came at about 180C. frown an oil change is in order...
 
 
 
 
    Rhodium
(Chief Bee)
05-23-03 16:34
No 435051
      Amination  Bookmark   

The most bogus step is very likely the (Delepine) amination... Hexamine amination of a secondary halide is unprecedented in the literature.
 
 
 
 
    hypo
(Hive Addict)
05-24-03 00:58
No 435122
      hmm...  Bookmark   

but note that IudexK is using NH3 in a bomb (sort of).
egotrip is using the delepine: ../rhodium/chemistry /dmmda-2.html

in the book named after our friend orgy, i read something interesting:
"the yield of primary amine can be increased by using an excess of
ammonia (obviously) or by adding ammonium carbonate or ammonium chloride"
i figure the primary amine being a stronger base will liberate an NH3
molecule and be transformed in the unreactive ammonium ion. the HBr/HI
produced in this reaction should already do this to some extent, but having
an excess of ammonium can't hurt. nice. smile
 
 
 
 
    Glacial_Refluxer
(Newbee)
05-24-03 05:38
No 435160
      Swim shall give it a try  Bookmark   

That DMMDA-2 synth looks pretty simple, but swim got kind
of discoureged when Rhodium made the comment on the
hexamine amination.

2 questions:

Swim does not have fractional distill equipment, would
useing  straight parsley oil yeild anything if the synth is
not bogus?

Could i2 crystals be used in place of the sodium iodide?

http://markmlucas.com/images/invertabrates/goliath%202.jpg