>In a perfect world, drugs would be legal and easy to obtain, then NONE of us would
>be making any of these things.
Really? I disagree. Some of the chemists are here because they are interested in the chemistry and not interested in making any money.
>Was the peracetic acid solution added drop by drop or all at once under cooling?
It was sitting in the fridge and them poured into the flask.
>Was the amination done under stirring?
Yes. The epoxidation, rearrangement, distillation and amination were all done with magnetic stirring.
> Btw, I don't really understand RoundBottom's post. What is the purpose of applying
>the vacuum for 30 minutes? Why not just stir the KOH and alkene for 20 hours at a
>temp of 160 instead?
That's what he does. The initial vacuum is to remove the water present in the KOH, otherwise you're
not going to affect the conversion of safrole to isosafrole and you risk destroying the safrole.
>Could you please just state what YOU did to make things easier.
I recited the general technique in other posts. Freezing and isomerization is hardly rocket science.
>Please include all weights and measurements. RoundBottom's diagram was just plain confusing to me.
Get him to clarify it then.
>What are the ratios of methanol/MeNH2-HCl/Al/ketone and how long did the reaction
>last before it was time to process the final product?
It went 5hrs.
The reaction details are novel, and are a combination of a variety of information already publically available. No synthesis that I could find uses prepares HOOAc from H2O2/acetic acid and does the oxidation in DCM (to the best of my knowledge). If you want my references for this reaction, I invite you to read:
EP patent 1,140,788
http://l2.espacenet.com/dips/viewer?PN=EP1140788&CY=gb&LG=en&DB=EPD
(pg27)
J Chem Ed, Volume 73 (6), 555 (1996)
https://www.thevespiary.org/rhodium/Rhodium/chemistry/2-phenylpropanal.html
US patent 3,028,398
http://l2.espacenet.com/dips/viewer?PN=US3028398&CY=gb&LG=en&DB=EPD
Organic Syntheses, CV 4, 860
The amination was:
133mmol mdp2p in flask A. 29.8g MeAmCl + 30mL water in flask B. 53ml water + 17.7g NaOH in flask C. In an ice bath, flask C is added to flask B. In a 500ml flask 185ml MeOH, 0.1g HgCl2. Stirred. Added 11.9g Al foil. Left stirring until it starts to bubble. Added flask B then flask A. Rinsed flask A with 10ml MeOH, added to rxn. Let run 5hrs. Basified with 89g NaOH in 210mL water. Extracted with 250ml toluene. Washed with 250ml 5% NaOH. Filtered toluene to remove chunks of foil. Washed with 250ml 5% NaOH. Washed with brine. Extracted with acidic water (titrated to pH 4). Washed with acetone. Took yield. Then went on to recrystallize. (no A/B or freebase distillation was done, I'm sure Rhodium & Osmium disapprove!)
If you need more details, read up more. I think all the essential details have been covered in these posts.