(too old to reply)
NEW PHENYLACETONE SYNTH HELP
Zaltar
2005-12-11 20:13:49 UTC
Im busy with a new synthesis for the Meth & Amphetamine precursor
Phenylacetone /

Phenyl-2-Propanone / Methyl Benzyl Ketone. Recently I found out that ( some
? ) Paint-Thinner

contains 2 ingredients:

Toluene or Methyl Benzene

Butyl Acetate.

On Rhodium Drug Archive there is a synthesis using Ethyl acetate and
Benzylcyanide in the P-2-P section.

This Reaction is very intresting for a new synthesis using Toluene and Ethyl
acetate. First look at the original

reaction !

1 Benzyl Cyanide + Ethyl Acetate + Sodium Ethoxide =
Alpha-PhenylAcetoacetonitrile

2 Alpha-PhenylAcetoacetonitrile + H2SO4 = Phenylacetone

What will happen in the reaction in practice is that in the first step a
crystaline mass is produced and this is acidfied

with acetic acid in h20 to seperate the Alpha-PhenylAcetoAcetonitrile out
from the crystals.

In my own experiment with Toluene instead of Bezyl Cyanide the crystaline
mass is produced. I dissolve these cristals

in 8% Acetic acid , but no Phenyl-2-Acetone will form, Why Why Why ?

Ph-CH3 + CH3COOCH2CH3 + Strong Base = PhCH2COCH3 + OHCH2CH3 or what ?

Is 8% Acetic Acid not strong enough ?

any help with this project or what,

THANKS FOR THE SUPPORT

ZaLTaR
j***@earthlink.net
2005-12-16 21:05:28 UTC
try benzaldehyde(bitter almond oil is 95%) + MEK =P2P
rocky
2005-12-21 21:02:53 UTC
UH J can you give short string of reaqctions? also a caution that
commercial methyl ethylketone is not 100% pur ealso; pure bitter
almond oil is hard to find (havent checked grocery store yet) better
yet conductin the reaction in alchol solevnt would be a plus ase you
won't have to frac. distill the commercial bitter almond oikl to clear
the ETOH.

IF it were that simple benzaldyhyde + MEK = P2p it would have been
written up long ago. ; but then a large # of SWIM's used mercury
instead of aluminium to reafct P2P and poisioned watersheads = so I
don't thing were the smartest bunch of grapes out there
Cooker
2005-12-22 14:11:21 UTC
Rocky...
how u been Bro...

it does work..the patent was posted at the hive in 1999 by twodogs...
cassia-reacts with a base->benzaldehyde..
Cinnamon oil -> benzaldehyde..


An acid catalyzed Aldo Condensation, followed by a Bayer/Villager,
peracid, eventually gives yield of

P2P.

The literature is well documented, and verified by many former
researchers. >)



MEK+Benzaldehyde--->MethylPhenylButanone


this can also be done with Acetone and benzene,.....bujt that is
another subject..

1) An acid catalyzed Aldo condensation of Benzaldehyde and Methyl Ethyl
Ketone to give Methyl Phenyl

Butenone ie C6H5CHO + CH3CH2COCH3 + dryHCL ---> C6H5CH=C(COCH3)CH3

2) The unsaturated ketone undergoes the Baeyer-Villiger oxidation with
peroxy acids to give the enol

ester of Phenyl propanone ie C6H5CH=C(COCH3)CH3 + RCO3H ---->
C6H5CH=C(OCOCH3)CH3

3) The enol ester is then saponified with 10% NaOH solution to give
Phenyl Propanone in about 35% yield

based on the unsaturated ketone.

yields will increase with a few little changes...
rocky
2005-12-28 21:10:46 UTC
Tha acid Aldo conversion is it done at pressure to keep the dryHCl
liquid or do you just use as gas at STP: tghe idea of keeping/having
dry 100% HCl at pressure as a liquid is well unsetteling

Thanks; but I'll stuck to fractionally distilling the bitter almond
oil; I DID see the acetone benzine as another potiential source; 3
astep process; All this effort because they pulled PPA(PPA is final
desiredd vet substance desiredc) as a decongestant/antihistimine in the
US. The perscription Entac(200mg PPA) or coricidean OTC(PPA 25mg) were
the ONLY meds I could take for a cold qand NOT have bad interactions
with the amps they give me for narcolepsy.

I need to put my searching hat on; finding biotransform(yeast)
coinversion to an intermediate and then steam extract and final step to
either P2P(acaqdemic; it's controlled) or PPA to clear my cats sinus
problems. I've received the intermediate name on the bromo fly thread.
that looks like a wank; good reports on the pure japanese product and
then(surprise; a US gakked up knok off that wont give a fly a headaCHE
OR VISIONS ETC)

tHANKS FOR YOUR EFFORT;L
INCIDENTIALLY THE LAST STEP; SAPONIFICATION WITH nAoh. Never really
thought of prop dope coming from a type of soap. And I thought Mr.
Clean only used ammonuia and sodium!!

incidentially; new pills have teh amine rather than suzy or eppie; any
dreams about the next step to create an MAmp anal..
Cooker
2005-12-29 13:51:27 UTC
the aldo can be done by refluxing Hcl or sulfuric acid also...is a very
easy process..
Zaltar
2005-12-31 21:52:58 UTC
Ey,, It seems all of you have some more skillZ in practice, but please help
me out, First of all
where the heck is my original post, but what the heck,

Im busy with a new Phenylacetone Amphetamine synth and it works qua theory,
well I think, but
first I want to keep it a secret until the hive is back on line, but because
I need to know what I do
wrong, thus I want to share it in this new year !

The first reaction go's like:

1 C6H5CH3 + 1 CH2COOEt >> NaOH / NaOEt >> C6H5CH=C(CH3)ONa

This is the synth where I get tha Idea from:

http://www.orgsyn.org/orgsyn/prep.asp?prep=cv3p0016

When I'm doing this reaction for real then I't seems to go ok: First the
reaction mixture is put
on slight heat , after several seconds the solution turns into a gelly
substance and then crystals
form when cooling down in freezer. Ok, then the step to phenylacetone: The
crystals are dissolved
in cold water and then a diluted solution of H2SO4 is added, This will
perticipate the P-2-P. Ok
dissolving the crystals was no problem and adding H2SO4 was also no problem,
then some sort of
white / yellow foamy foam perticipate's, this foam dissolves into organic
solvents, I's this P-2-P ifso
then why is it foam or is the P-2-P in the water mixture ? Maybee I fucked
up somthing so
I thought maybee the crystals are ok but maybee I did something wrong, so I
thought, when looking
at those nice powdery crystals, hey, maybee this could be a new drug
precursor if it was possible
to convert it directly to Amphetamine ! Well:

1 C6H5CH=C(CH3)ONa + 1 NH4Cl = 1 C6H5CH=C(CH3)NH2

then you only have to saturate the double bonded intermediate and you
probebly have Amphetamine??
Also How stable is that intermediate C6H5CH=C(CH3)NH2 ?

I NEED some help, but anyways I do some tests, and if you think , hey this
could be something, mail me and you get my research work on this topic !

Thanks , bye , Tha Snitcha !
Post by Cooker
the aldo can be done by refluxing Hcl or sulfuric acid also...is a very
easy process..
Cooker
2005-12-31 23:19:17 UTC
interesting..
Zaltar
2006-01-01 14:08:40 UTC
The Rompas Condensation:

C6H5CH3 + NaNH2 = C6H5CH2Na
C6H5CH2Na + CH2COOCH2CH3 = C6H5CH=CH(CH3)ONa + EtOH

EXPERIMENTAL SYNTHESIS:

18gr Sodium amide is suspended in ~120ml Ether and is stirred at roomtemp.
Introduce by
dripping in, 92.14gr Toluene after addition is complete the solution is
stirred for 30min. Then
was add dropwise 88.10gr Ethyl Acetate to the reaction solution and keeping
the temperature
as low as possible. After addition is complete, the whole is stirred for
another 2~3 hours at room-
temp. Then the solution is put in the fridge over night. The next morning a
crystaline mass is
formed in the solution. This is filterd out of the solution and the
filtercake is washed with more
ether. The crystals are air dryed. You now have the P-2-ONaP precursor.
Zaltar
2006-01-01 14:25:37 UTC
Amphetamine from P-2-ONaP ?????

When P-2-ONaP is reacted with Ammonium Sulfate then the imine will form
witch cann be
hydrogenated by your own chosen way to get a a-Methyl Phenethylamine or
Amphetamine.
The reaction to amphetamine's cann be done without isolating the formed
imine and is
investigated.When doing very large scale industrial synthesis you may find
it more
practical to isolate the intermediate but pure imine is readly unstable if
it come's in
contact with water.

Imine formation and reduction.

The best way for imine formation are anhydrous conditions. Dissolving you
crystals in
EtOH at roomtemp then the conversion to imine followed by reduction with
NaBH4 is
one good way to produce high yeilds of amines. The formation of imine must
be performed
in an anhydrous solvent such as MeOH / EtOH. Use Ammonium sulphate as the
reaction
reagent because the Na2SO4 generated in the reaction is used directly as an
drying agent.
Ammonium Chloride should also work , but the formed water forms a problem
with the
imine so much lower yeilds cann be expected.

Tha Snitcha aka ZaLTaR
nuclearchick
2006-01-07 07:01:13 UTC
I see SWIM everywhere I read, what does it stand for? Please pardon
the intrusion, I'm still a newbie. Thx.
~xy~
2006-01-07 18:33:13 UTC
S omeone
W ho
I sn't
M e
nuclearchick
2006-01-09 01:14:00 UTC
Ha!! Thats funny! Muchas gracias!
~xy~
2006-01-09 01:18:07 UTC
de nada
nuclearchick
2006-01-09 01:30:41 UTC
Ha! thats funny! Muchas gracias!!!!
Cooker
2006-01-09 08:40:57 UTC
SWIM is the best underground chemist ever...SWIM says that u are polite
Cooker
2006-01-09 09:18:15 UTC
Zaltar...won't work buddy
nuclearchick
2006-01-09 16:11:00 UTC
well I try.....
m***@hotmail.com
2014-04-23 04:40:27 UTC
Post by Zaltar
Im busy with a new synthesis for the Meth & Amphetamine precursor
Phenylacetone /
Phenyl-2-Propanone / Methyl Benzyl Ketone. Recently I found out that ( some
? ) Paint-Thinner
Toluene or Methyl Benzene
Butyl Acetate.
On Rhodium Drug Archive there is a synthesis using Ethyl acetate and
Benzylcyanide in the P-2-P section.
This Reaction is very intresting for a new synthesis using Toluene and Ethyl
acetate. First look at the original
reaction !
1 Benzyl Cyanide + Ethyl Acetate + Sodium Ethoxide =
Alpha-PhenylAcetoacetonitrile
2 Alpha-PhenylAcetoacetonitrile + H2SO4 = Phenylacetone
What will happen in the reaction in practice is that in the first step a
crystaline mass is produced and this is acidfied
with acetic acid in h20 to seperate the Alpha-PhenylAcetoAcetonitrile out
from the crystals.
In my own experiment with Toluene instead of Bezyl Cyanide the crystaline
mass is produced. I dissolve these cristals
in 8% Acetic acid , but no Phenyl-2-Acetone will form, Why Why Why ?
Ph-CH3 + CH3COOCH2CH3 + Strong Base = PhCH2COCH3 + OHCH2CH3 or what ?
Is 8% Acetic Acid not strong enough ?
any help with this project or what,
THANKS FOR THE SUPPORT
ZaLTaR
9 years old this post,,,,toluene has 1 methyl group on the benzene ring witch is not reactive with that syth,,benzylcyanide has a CN BONDED TO the methyl group in this syth it is the cn bond witch attacks the acidic acetate,,
,toluene is a Bummer the only synth iv had use for it is the chloroacetone and aluminium chloride refluxed with toluene witch form 4-methyl-1-phenylproan-2-one,,witch is phenylacetone with a extra methyl group other side of the benzene ring