report: small PMP-2-P synthesis

[pyroflatus]

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.
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.