Author Topic: report: small PMP-2-P synthesis  (Read 950 times)

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pyroflatus

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report: small PMP-2-P synthesis
« on: January 11, 2004, 06:48:00 AM »
This is a report of a small scale PMP-2-P synthesis inspired by Chromic.

1) Illicium verum oil was fractionated at atmospheric pressure to yield ~50g Anethole.
2) 14.8 g anethole was mixed with 50g CH2Cl2 and buffered with 7.5g NaHCO3 and epoxidized with 39g performic acid. Reflux condenser was attached and no cooling was applied bar initial cooling of reactants/solvents to ~0°C
3) Reaction was run for 5 hours (exothermic reaction completed at 3.5 hours)
4) Organic phase was extracted with 2x30mL CH2Cl2 and combined extracts washed with 2 x 30mL 5% NaOH soln.
5) solvent was stripped and glycol/epoxide refluxed for 2.5 hours with 200g 15% H2SO4 with ethanol as per

rhodium's site

(https://www.thevespiary.org/rhodium/Rhodium/chemistry/peracid.html) (substituting ethanol for methanol)
6) organic phase separated and aqueous phase extracted with 2x30mL CH2Cl2
7) Aqueous phases backwashed with 2x30mL CH2Cl2 and organic phases combined.
8) Organic phases washed with 2x 30mL 5% NaOH soln. and 30 mL NaOH conc. coln.
9) CH2Cl2 stripped and ketone distilled at 400mmHg (235mmHg at pump) 76-78°C resulting in 9.82g PMP-2-P

Sodium metabisulfite test on suspected ketone resulted in white crystals.
PMP-2-P has an agreeable MDP-2-P-like taste, but very little smell, with no anise component to the scent.

Now on to isosafrole/MDP-2-P.
When both ketones are complete, reductive amination with methylamine and hydroxylamine is planned, with intended production of p-MA, p-MMA, MDA, MDMA.

NB: I think small insufflated lines of pMMA.HCL are an entertaining adjunct to alcohol consumption. Alone pMMA results in a nostalgicly pleasing "fucked up on drugs" feeling without noticeable negative side effects.