P2P to (d)-Phenyl-2-propanol Possible?

[Acab1312]

Hello I have seen a P2NP synthesis that mainly produces the d isomer. Wouldn't it then be during the conversion to P2P to take over the D product?

 

[OrgUnikum]

Thats an interesting one, I have not known this, cool! It is of course not P2NP what is made but it has a alcohol group added on the first carbon, it is the direct precursor to Norphedrine as P2NP is the direct precursor to Amphetamine.

This means you need some heavier guns then NaBH4/CuSO4 to get d-Amphetamine, of course RP/H3PO3/H3PO2 + I or the Birch will do the trick, some other methods come to mind.

But I have not the slightest idea why the condensation of benzaldehyde with Nitroethane with triethylamine as catalyst results in the nitroalcohol and not the nitro-only-compound as known. Also why it is selectiv not only for cis or trans configuration, thats also a surprise. Strange.

 

[K-Cyanide]

The topic is also of great interest for me, though from a different point of view. The resolution of racemic methamphetamine free base can be done without solvent through my favorite compound (grin):
O,O`(+)-dibenzoyl-d-tartaric acid in good yields. (80-85% ).

However, i wanted to ask if anybody has expierence with the so called RRR-process. RRR stands for resolution-racemisation-recycling, to re-racemise the unwanted l-isomer back to a 50:50 racemic mixture. This is conducted using small amount of a radical initiator like AIBN and a source of thiyl radicals (ie methyl thioglycolate). This way one can drive up yields from theoretical 50% to over 90% by running the process several times. I couldn´t find any reasonable procedure write down so far.

 

[花谢花开]

Which dibenzoyl tartaric acid do you use to split cas? Is it the liquid part or the crystal part? Can you explain it in detail? I agree with this method. I think it's better than tartaric acid. Thank you.

 

[OrgUnikum]

This is what you need to know....

Optical Resolution of N-methylamphetamine Via Diastereoisomeric Salt Formation With 2R,3R-O,O´-Di-p-toluoyltartaric Acid
DÁVID KOZMA, ZOLTÁN MADARÁSZ, CSABA KASSAI, AND ELEMÉR FOGASSY
Department of Organic Chemical Technology, Technical University of Budapest, Budapest, Hungary
CHIRALITY 11:373–375 (1999)

 

[OrgUnikum]

Dutch resolution and a lot of other stuff regarding all this good explained:

RIJKSUNIVERSITEIT GRONINGEN

Resolutions of Racemates by Crystallization
Additives and Attrition
Proefschrift

 

[Acab1312]

Maybe this will help you further I have not tested it personally yet. I could look in my folders maybe I can find the original PDF still

General Procedure for the Racemization Experiments. A
0.06 M solution of amine (100 mg) and thiol (1.2 or 0.2 equiv)
in benzene was refluxed for 2 h (stoichiometric condition) or 7
h (catalytic condition) in the presence of AIBN (an overall
quantity of 20 mol % of AIBN was divided into three equal
portions (when reaction time > 2 h) that were added succes￾sively each 2 h). After concentration, the residue was diluted
with HCl (1 M), and the solution was washed with Et2O. The
aqueous phase was basified with saturated sodium carbonate
and extracted with Et2O. The pure amine was isolated after
drying on MgSO4 and concentration

 

[Sciencenutz]

I have access to aibn and thiol but would appreciate some help with the proper ratios converted to say per kg of L-meth freebase? I'll post my results

 

[Sciencenutz]

Any updates on this?

 

[K-Cyanide]

I think I will join the young research team and will also do some experiments. .
In order to get started i have to procure the compounds Methyl-thioglycolate and the funny compound AIBN. I always check the big chem companies to have an estimate of the costs. (by dividing their price by 5 grin). Any hint for reliable supplier is appreciated.

Regarding solvent i noticed on Sigma-Aldrich and several other sites, they sell 0.2M solutions in Toluene, so actually Toluene seems to be a proper choice.

​

 

[btcboss2022]

I Have supplier for AIBN and thiol if needed.

 

[Acab1312]

Hello how high would the price be with your supplier, When it comes to the experiments, I also agree with.

 

[btcboss2022]

Not high last time I asked was around 500€ the moq of both shipping included.

 

[K-Cyanide]

ok sounds reasonable, what is the moq, 1 kg I guess. And what about lead time, from the time the payment is received by the supplier?

 

[btcboss2022]

1kg each 15 days delivery.

 

[K-Cyanide]

final question, do they accept cryptocurriencies, though if not, that wouldnt be a no deal reason at least for me. thx

 

[btcboss2022]

Yes they do.

 

[K-Cyanide]

perfect, then please provide us with contact data. Here, or if privacy is a concern via PM.Thank you very much.

 

[btcboss2022]

Let me ask them how they prefer to do it.

 

[btcboss2022]

I will talk with my supplier today and they told me that they don't have enough time to manage forum deals they asked me to act as man in the middle so...tell me your opinion about this.
I thought the option to ad their main products here and I would manage the deal directly with a little comission in price obviously ;-)

 

[K-Cyanide]

The process is basically fine, including a commission for you. The most important question here is how the sensitive data is handled. Would you then send the packages to the end customer or the supplier directly from China?

 

[btcboss2022]

Is sent by supplier not me.

 

[K-Cyanide]

ok, so let me know if they agree. Another brief off topic question: Do you use a heater/chiller for your reactor or just a heating unit? And which coolant / heat transfer liquid are you using?

 

[btcboss2022]

I have a heater/chiller unit and a bath oil is used as transfer liquid.
If they are agree?What you mean?
Thanks.

 

[K-Cyanide]

Well, then I suggest you to collect orders from the guys who wanted these reagents (including me) and then you order it with your supplier.

 

[btcboss2022]

Yes that is what they told me.