Below is the procedure to convert Pseudoephedrine/Ephedrine to P2P, from Rhodium archive;
Quote
When ephedrine and related compounds are heated in strong aqueous acid, they are dehydrated to the enamine, which spontaneously can rearrange to the isomeric imine (Schiff Base), which then can be hydrolyzed into phenyl-2-propanone and an amine salt. As all the steps are reversible processes, the reaction equilibrium is driven towards the desired product by continuously removing the formed phenyl-2-propanone by the aid of steam distillation.
Ephedrine derivatives that can be used in this procedure include Ephedrine, Pseudoephedrine, Norephedrine and Norpseudoephedrine (Phenylpropanolamine). Many other metal salts can be used instead of the zinc chloride.
1025g 75% sulfuric acid was mixed with 1g ZnCl2, and 192g (1.16 mol) Ephedrine or Pseudoephedrine freebase was dissolved at a temperature of 50-100°C, and the reaction mixture was heated further to 145-150°C. At 125°C steam is passed through the solution to facilitate mixing of the contents. At 145°C the stream of steam is increased, and during 2.5-3 hours the phenylacetone is steam distilled from the reaction mixture. The the crude phenyl-2-propanone, which is free from propiophenone, is isolated by toluene extraction of the distillate. After distillation through a short vigreaux column, 130g (82%) of phenyl-2-propanone is isolated in a purity of 99.8%.
Basically the procedure above is one pot 2 step from pse/e to p2p, 1st step is dehydration pse to imine and 2nd step is imine hydrolysis to p2p and methylamine.
If 2nd step is not performed, imine is gotten, imine is known very easy to reduce/hydrogenate, moreover if compare to damn hydroxyl group.
So, the procedure from pse to meth may be something like;
1. Pse dehydration to imine,
By strong acid like h2so4 or h3po4, 98% or more considering imine is very sensitive to water.
2. Imine reduction/hydrogenation
May be by neutralized H2So4 with metal like zinc, in anhydrous alcohol, the flask is in ice bath. Or neutralized by anything that wont produced water, methylamine freebase?
Filter and then reduce by nabh4.
But if possible, another reducing agent instead of nabh4, an otc one. Will be very interesting if Sodium dithionite (Na2S2O4) can be used as reducing agent (like in Rhodium archive).
Notes;
1. 85% H3po3 is heated to almost anhydrous, can be done by heating it at temperature just above 149 c. pse freebase is added, stirred well, heat 80 c for 12 hrs.
Anhydrous IPA and urushibara nickel is added, reflux for 4 hrs. Extract the product, no oil is occurred when basify, solid freebase only, means the pse didn’t converted to enamine.
2. 85% h3po4 is heated to almost anhydrous, pse freebase is added, heat 149 c min for 3 hrs. Some precipitation is occured.
Anhydrous IPA and urushibara nickel is added, reflux for 4 hrs. 2 kind of product is obtained, one has a lower melting point than another, both are not pseudo (but it cant use as conclusion). So, pse dehydration by h3po4 should be performed at temperature above 149, and may be for 5 hours at 149c, or 3 hours at 160c, just maybe.
Every feedback will be much appreciated, about how to do, chemicals that should be used, even you can prove that this idea is only good on the paper