09-18-03 07:45
No 459701
after big heating of the aldehyde and alanine, dark brownish/redish sticky goo remains smelling nothing like the aldehyde. Addition of h20 to the flask - the sticky stuff is not very h20 soluble, but upon heating, seems to take up enough of something to turn it a sun yello. Goop still coats flask.
Evaporation of the yello h20 and acetone crashing at the tail end results in lots of what appears to be alanine based on quantity/crystal reflectivity, smell. SWIM will decant crap from residual alanine before trying all this again.
goop in flask taunts swim, so he thinks ghetto like, and decides to try a 3 solvent extraction:
50:50 acetone and h20 is added to the remaining goop - it dissolves easily with minimal heat and swirling, turning bisolvent dark red. Addition of tetrachloroethylene and swirling with a little more heat resulted in a very dark red lower layer (tetra) with a yellowish white upper layer, which intensifies in color as low heat is applied for about 10 minutes. SWIM is hoping that this means that more of the hopeful PPA is in the h20 layer because the goop was thinned considerably. Will evap the top layer stuff and post results later.
any knowledge a bee wanna drop on a newbee would be nice.
(Hive Bee)
09-18-03 21:57
No 459797
Hmmm, doesn't it have to be decarboxylated befpre forming PPA? Also, if the PPA is in freebase form, maybe adding H2O to the goo and steam distilling?
SWIM wants to experiment with this method, but is thinking of saying "fuck it" and synthesizing nitroethane. If SWIM does that, then the bisulfite of the aldehyde will be reacted with EtNO2, and the nitropropene formed reduced giving PPA. SWIMS has dreams of P2P and 4-MAR from the PPA!
(Newbee)
09-19-03 00:26
No 459813
did the condensation rxn with nitromethane, bzh, and naoh in methanol. very exciting visually, then swymhm realized that the outcome would be phenethylamine...
(Hive Bee)
09-19-03 00:47
No 459816
Nitroenthane not methane, so the outcome is an amphetamine.
(Active Asperger Archivist)
09-19-03 08:31
No 459895
We need a "bitch-slap" button for the newbees. Just so it complements the "UTFSE" comment. What do you think you can do to help work this one out?
Act quickly or not at all.
(Newbee)
09-19-03 14:30
No 459943
It's my current understanding that heating benzaldehyde with alanine causes decarboxylization of the alanine once the temperature rises high enough.
(Active Asperger Archivist)
09-19-03 15:47
No 459951
does not occur like that. The two substrates first react in a condensation reaction (I believe- it's in one of the many papers I've posted in the digest on Ephedrine under the AKABORI section- HINT, HINT, HINT....)
Once the two have united, then the mix is heated to the point of decarboxylation of the product formed in the previous step.
Act quickly or not at all.
(Hive Bee)
09-21-03 05:42
No 460180
does not occur like that. The two substrates first react in a condensation reaction (I believe- it's in one of the many papers I've posted in the digest on Ephedrine under the AKABORI section- HINT, HINT, HINT....)
Once the two have united, then the mix is heated to the point of decarboxylation of the product formed in the previous step.
Yes, see thats what I was talking about. And yes, the AKABORI thing I've read before, where they talked about using serine and shit. Interesting stuff!
(Hive Bee)
09-21-03 20:24
No 460251
Yeah SWIM did another search on AKABORI last night, very cool stuff! SWIM will try the condensation with glycine, followed by the acid hydrolysis to 2-methylphenylserine. The only problem will be decarboxylation to PPA. But SWIM will work on it, and doesn't really care about low yeilds. SWIMS got plenty of toluene to twerk benzaldehyde from and glycine is a very cheap amino acid. Plus since SWIM has dreams of making phenylacetone from the PPA, chirality isn't an issue.
Quick question about chirality. When SWIM was looking at some pics of structures to amino acids, the solid looking triangle means it's pointing toward you, and the striped away right? Or is it the other way around? Also, which is the levo isomer, pointing toward or away?
(Active Asperger Archivist)
09-22-03 05:16
No 460314
If you're using glycine, where's the extra carbon coming from to form PPA? (HINT: you need alanine.)
Act quickly or not at all.
(Hive Bee)
09-22-03 21:11
No 460425
Oh yeah your right, I misread a few things thats all. Thats good then, because decarboxylation will be easier.
(Hive Bee)
09-23-03 12:07
No 460530
a simple way for decarboxylation:
Patent DE389881
(Hive Bee)
09-26-03 02:58
No 461101
Can anyone translate the german please?
(Hive Bee)
07-09-04 23:42
No 518446
Amalgam ...... did you ever get the patent DE 389881 translated? If so what are the chances of getting a copy.....? As I have been looking at methylating the alpha carbon of Phenylalanine then decarboxylating it to get to amphetamine. I'm getting tired of working on the COOH part of the molecule , so it's time to change the strategy.........java
Just hold on to the thread...that keeps us going
http://www.chiapaslink.ukgateway.net/