Can anyone tell me if this recipe is viable? Apparently it is very easy and does not require special equipment...

[84modfo3j]

(First of all, I am a total noob. The biggest recipe I've ever made is to make myself dinner)

you can find it by searching "Method for making phenylethylamine compounds EP2540698B1"

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Example 1 Dextroamphetamine (not according to the invention)

• [0028]
  A mixture of 6.00 g (33.9 mmol) (4S,5R)-(-)-4-methyl-5-phenyl-2-oxazolidinone, 0.34 g 10% palladium-on-carbon (50% water wet), and 60 mL SDA-3A (a solvent constituting 95% Ethanol and 5% Methanol) was stirred under a hydrogen filled balloon at ambient temperature (approximately 20°C) until no more oxazolidinone was detected by HPLC, 4 h. The reaction mixture was then filtered through a pad of Celite to remove the catalyst. For the purposes of isolating the free base, a filtered reaction mixture was carefully concentrated under reduced pressure to leave 4.47 g of a crystalline semi-solid, which was found to be a mixture of 96% dextroamphetamine and 4% ethanol by 1H NMR. Some dextroamphetamine was detected in the distillate. Yield = 94%. 400 MHz 1 H NMR (CDCl3) 7.34-7.20 (m, 5), 3.22-3.17 (m, 1), 2.76-2.72 (d of d, J = 13.2 Hz, J' = 5.4 Hz, 1), 2.57-2.52 (d of d, J = 13.2 Hz, J' = 8.1 Hz, 1), 1.16-1.14 (d, J = 6.3 Hz, 3).

Example 5 Dextroamphetamine Sulfate

• [0032]
  The method of Example 1 was followed until the catalyst was filtered away whereupon a total of 7 mL 25% H2SO4 (aq) was added dropwise to the filtrate over 3 min. After cooling in an ice/water bath for 15 min, the mixture was filtered to collect the dextroamphetamine sulfate using cold SDA-3A as a flask and cake rinse. After drying, a total of 5.79g of dextroamphetamine sulfate was obtained, 93% yield. This material was assayed at 100% by HPLC.

what meaning that "not according to the invention"????

this could be done? Has anyone tried it? Seems too easy to be true, doesn't it? Someone could make a new recipe explained for "Noobs".

If I understand correctly, you basically wouldn't need any excessively rare or expensive equipment... and all materials are easy to acquire.

Is this recipe something hidden and not exploited by most? I can delete the post if it bothers someone ^ ^, just say it

 

[OrgUnikum]

Never seen this before, but it seems genuine and with the dimethyl variation of the starting compound one gets d-Meth.
Lookchem says the industrial production of the precursor has just started, but by now the cheapest offer is something like 600 USD for 100 g what would be a bit steep.
Doing it as CTH would eliminate the need for a hydrogen gas bottle, i is nicely with references in the patent:

US20100125146A1 - Method for making pharmaceutical compounds - Google Patents

A method of making a phenylethylamine of formula B: wherein R 2 , R 3 , R 4 , R 5 , R 6 , R α , R β and R n are each independently selected from hydrogen, alkyl, acyl, aryl, amido, amino acids, sugars...

patents.google.com

I am quite sure one could do this also with RP/I (or H3PO3 or H3PO2 and Iodine) or the Birch.

I am curious how the (4S,5R)-(-)-4-methyl-5-phenyl-2-oxazolidinone is synthesized.

That this is not used comes from the unavailability of this precursor or its unavailability at a reasonable price. And I bet it will be not available for very long as soon it hits the market

For somebody who does not know chemistry I think HI, Phosphorus compound and Iodine would be the most promising method, hydrogenations are a bit tricky and catalyst re-usability is questionable when standard Pd/C is used.

Very interesting, thanks, sorry that I can offer only mostly guesses.

 

[84modfo3j]

i read on theehive in reddit that it was arround 1000USD/Kg (2 years ago) from china "if you have connection".


i just ask for price out of curious a bunch of random emails from lookchem and chemicalbook (just random, not trusted...) and get arround 250gr/700usd - 1kg/1700USD... (at 95% aprox yield.. looks not too bad to me, but i don't know at what price you can get/cook other precursors like P2P..) they seems to have it in stock.. i will ask for free sample to see if i have luck


how you know/ why you think "the industrial production of the precursor has just started"? you mean this year? and why you think it would not be aviable? if there is demand- there will be offer i think..


just find a short talk about this process also on theehive:

Process: 4.5 hrs hydrogenation at atmospheric pressure (to us that's the biggest fat Toys'R'Us balloon filled up with Hydrogen gas 5.0. Balloons sacks down 10-15% every 7-12 minutes some 13 to 18 times, fill it up again to max with H2, when balloon doesn't sacks down no more the reaction is over. Takes 4 to 4.5hrs at 500 gram batches. This method doesn't run faster under higher pressure, balloon / 1 atm. is fine.


as i have no idea what i (and you) are talking about, i don't know how CTH is made. that process is dangerous/generate heat? I still have to investigate a lot. But this process catches my attention because it is apparently less dangerous than the "conventional", more efficient and faster. If one day I get the precursor I will ask again in the forum or try to look for a mentor



sorry for my english and thanks for read.

 

[OrgUnikum]

I know about the industrial production having started because Lookchem tells it frankly on the compounds page. Prices should quite soon drop considerably.

You cannot go after yields named in patents, articles or writeups. I am sure though that they are quite high, something between 80% to 90% should be well in reach. Your 95% are a pipedream only to reach by self-deception, the starting material has 98% - claimed. There are always side-reactions and mechanical losses too, so 95% "yield" could only be done by omitting proper post-reaction workup and imagining everything what is a base coming from the reaction is "product". But a very good workup is necessary for hydrogenations as those can and will form byproducts, not a big amount usually but often the nasty kind, say byproducts which are active in themselves, just not in the wanted or generally healthy way.

Running this with a balloon and 500 g + is utter nonsense, search for "Parr shaker" and look at the setup. You use something like a propane bottle as intermediate hydrogen storage, the pressure for this to have the eact amount of hydrogen needed can be calculated and then this vessel is charged and it feeds the reaction vessel per pressure reducer with say 1,5 to 3 bar constantly. When the pressure in the whole systen has equalized at a known number it is done. This calculation was the hardest thing back then when I did this. Otherwise Pd/C can reduce a lot more then just what you want it to reduce and having it stop at the right point without precise calculation is a gamble.
CTH with some formate as hydrogen donor is far less demanding here and also the calculations are much easier.

One point before I forget it: You want to shake the reaction not stir it. Reason is simple: Stirring atomizes Pd/C into ultrafine virtually unfilterable particles, shaking keeps more or less the original particles intact, they are tiny enough to be a pain in the ass, you always need Celite as filter-aid to stand a chance.

Almost no special laboratory equipment is needed but some workshop skills and equipment should be available. Much can be done astonishing simple, for example I had the reaction vessel on a skateboard which was moved back and forth by a windshield wiper motor from a car and some springs on the other side. This jerked the vessel back and forth providing exactly the kind of shaking ideal for this kind of reaction. Worked really well, if I ever do it again I will do it like this.

 

[Osmosis Vanderwaal]

Not a snowballs chance in hell.
Oxizolidinones are antibiotics. Here is a 2-d model of the chemical you name

You can get 5g for $70 from Sigma Aldridge, but hang on and I might be able to run that synth for you and tell you what you actually get

 

[Osmosis Vanderwaal]

63% chance of one of these

 

[84modfo3j]

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