11-14-02 06:56
No 379608
Hi
Due to the regulations with the chemical nitroethane, i decided to go about making 2,5-DMA with making 2,5-dimethoxyphenylacetone from 2,5-dimethoxybenzaldehyde with methyl 2-chloropropionate and sodium methoxide, the yeld from this is 14g.
Now, in order to make 2,5-dimethoxyamphetamines from this, is a simple P2P->amph reduction done the same way to make regular amphetamines from standard P2P on place to use here, or is prehaps the 2,5-dimethoxy group of a fragile nature that would require something else ? anyways, if u got any good ideas or simple reductions of 2,5-dimethoxyphenylaceone to 2,5-dimethoxyamphetamine, please respond.
Thanks
TreSprit
Chemical Generation
(Hive Bee)
11-14-02 07:09
No 379612
IŽd suggest you make the oxime from the ketone with hydroxylamine, then reduce the oxime to the amine with amalgamated aluminum in acetic acid. There are write-ups for both conversions here. If this route isnŽt useful for you then you need to specify which reagents you cannot get hold of.
Catalytic hydrogenation freak
(Hive Bee)
11-14-02 07:18
No 379617
Isnt the Leuckart reaction almost as high yeilding and somewhat easier?
Thats the route i would chose :)
(Chief Bee)
11-14-02 07:36
No 379621
No, the Leuckart reaction generally sucks.
Even this ( ../rhodium/pdf /leuckart.pdf ) Leuckart reaction review admits that phenylacetones usually gives a 20-70% yield, the substituted ones being in the low end. Don't even think about it.
11-14-02 09:29
(Rated as: UTFSE!)
(Hive Bee)
11-14-02 09:58
No 379654
UTFSE, perhaps....
Catalytic hydrogenation freak
(Stranger)
11-14-02 12:49
No 379696
2,5-DMA has been made from 2,5-dmp2np via the Leuckert rxn in ~60% yield.
(Bear With Me)
11-14-02 14:19
No 379738
Due to the regulations with the chemical nitroethane, i decided to go about making 2,5-DMA with making 2,5-dimethoxyphenylacetone from 2,5-dimethoxybenzaldehyde with methyl 2-chloropropionate and sodium methoxide, the yeld from this is 14g.
So you got 14g yield? That could be a 0.01% yield, or a 100% yield, for all we know. WTF amount did you start with?
PB
WARNING:The punishment for self-rating your posts is a slow and agonizing death!!!
(Stranger)
11-14-02 14:44
No 379751
16g of the benzaldehyde was used
TreSprit
Chemical Generation
(Hive Bee)
11-14-02 23:40
No 379898
2,5-DMA has been made from 2,5-dmp2np via the Leuckert rxn in ~60% yield.
To obtain amphetamines, Leuckart can only be applied on P2Ps, not P2NPs. Furthermore, I have very very high doubts that your 60% yield is a pure substance. In other words, I'm about sure that 50% of your 60% yield consists of useless molecules, most probably condensation products. Unless you show me a chromatogram demonstrating the high purity of your product, I cannot believe you
.Ave Hive, synthetisandi te salutant!
(Hive Bee)
11-15-02 04:41
No 379947
I have no idea about his end product but isn't melting point test enough to convince you that his yield doesn't have 20% of impurities?
(Chief Bee)
11-15-02 08:22
No 380000
What melting point? What writeup?
(Pioneer Researcher)
11-15-02 08:34
No 380008
If you have Pd/C from a commercial supplier, you can try the CTH reductive amination with am. formate in 1:9 water methanol and a 20-25 % of 10 % Pd/C, probably you'll get a 70-80 % yield. Check MDA and MDMA from CTH reductive amination, by Sunlight.
(Hive Bee)
11-15-02 09:19
No 380023
Maybe I should've formulated my post differently. I didn't mean there was evidence of a 60% yield nor a writeup to back it. My point was that asking for a chromatogram to prove purity to prove a yield is overkill.
(Stranger)
11-15-02 11:14
No 380057
13.41g 2,5-Dimethoxyphenylacetone and 50g of finely powdered calcium oxide is placed in a flask and heated in an oil-bath for a few minutes. Then 20.08g hydroxylamine hydrochloride is added, and the mixture is stirred with a magnetic stirrer in the presence of air for 1 minute at 130°C. Afterward, the reaction mixture is mixed with ethyl acetate, filtered to remove the calcium oxide, then mixed with water and extracted with ethyl acetate. The pooled organic phases is dried over Na2SO4, filtered and the solvent evaporated in vacuo to give 2,5-Dimethoxyphenylaceton oxime, i hope
At least if im not totaly wasted writbg down this, its based upon Rhodiums writeup for ketone->oxime.
His yeld was 1,49g, if this same reaction could be done to DP2P with simelar yelds, i chould have something like 14,9 of my oxime
Anyone ?
TreSprit
Chemical Generation
(Stranger)
11-15-02 17:08
No 380142
To obtain amphetamines, Leuckart can only be applied on P2Ps, not P2NPs. Furthermore, I have very very high doubts that your 60% yield is a pure substance. In other words, I'm about sure that 50% of your 60% yield consists of useless molecules, most probably condensation products. Unless you show me a chromatogram demonstrating the high purity of your product, I cannot believe you
I am aware that the Leuckert works with ketones not nitroalkenes. The dmp2p in the Leuckert rxn I was talking about was made from dmp2np w/Fe-HCl. The product was purified via standard a/b then vac. distilled. I didn't do a chromatograph or a mp test on the hydrochloride, and I don't really care if you believe me or not. I don't have a reference to back this up; I was simply offering information I know to be correct. IMO this is more valuable than a ref. for a procedure in a journal performed by research chemists, the yields in which are rarely reproducable by an amateur chemist.