What's the TEK for converting morphine --> dihydromorphine using Pd/C?

[Pikasso35]

I know I know, shame on me for asking for such a simple procedure but I just can't think clearly atm..

Starting from morphine, I know you need pure ethanol (simplest solvent) and Pd/C 5% or 10% for hydrogenation. Just forgot the actual step=by-step of it all:/

Sorry for sounding stupid...

Oh and can Pd/C 10% be used for hydrocodone --> hydromorphone conversion instead of Palladium Black?

[borohydride]

US Patent 6887999 is the simplest codeine->DHC hydrogenation. I've also posted reference to some SnCl2-based reductions.

Pd/C isn't used for hydrocododone->hydromorphone. HBr + H3BO3 is...

[PcChip]

He may have meant to type M -> HydroM / C -> HydroC

[Woody Bear]

The reaction that converts codeine to hydrocodone, and morphine to hydromorphone is written up here:
http://www.erowid.org/archive/rhodium/chemistry/dihydromorphinones.html

[borohydride]

Or, for 97% yield rather than the old (as per Woody's ref) 65% yield - US Patent Application 12/757,098

[duck]

BORO: I really enjoy.and read every one.of your posts.I think.it would be neat.if you would post a step by step thread about getting morphine from.pods. the only thing I struggle with is your posts are rarely organized well and they don't really read very well.

A good examplebwould be Woody Bear, when he explains synthesis stuff he breaks it down into a step by step process that is easy to read; im not busting balls, im just giving my input.because your knowledge is awesome, if only it could translate well to people who aren't so technically minded.

It seems like a lot of your posts get disregarded because they simply contain info that could be derived from a google search, whereas if we had a member from here whoncould organize that knowledge into useable processes here for at least some people here would be awesome.

Again, I hope you stick around and keep posting. You are very welcome.here. ever since we lost.our GEM of an anarcho Chemist, ROBOJUNKIE, the. Chem aspect of this forum has been on.the decline.

[Woody Bear]

Or, for 97% yield rather than the old (as per Woody's ref) 65% yield - US Patent Application 12/757,098
Here's a quote from the link I gave;


Example 6:

21 grams of codeine freebase was dissolved in an excess of dilute sulfuric acid, and two grams of palladium black was added and the solution refluxed for one hour. The yield was 90% of theory.
That and another one which quoted 85 - 95% yield were the best yields given, yields varied depending on the reaction conditions, but were usually around 75%. If you want high yields, then you have to follow the procedure exactly as it was done.

Borohydride is right that in the patent he gave which uses ruthenium does get a higher yield, however in order to get those yields the reaction needs to be done under nitrogen gas. Also the solvents and reagents are more difficult to get for the home chemist.

Anyone can buy palladium coins, so that is less likely than rare metal catalysts to become restricted, and every year, more and more chemicals become restricted and unavailable for the home experimenter to buy any more.

They are both good routes, the one I posted has slightly lower yields but is more OTC, borohydrides posted route needs more complicated equipment, and rarer solvents and reagents, but gets slightly higher yields.

Personally I like the ruthenium route, but I don't want to have to plonk down £300 for 5g of catalyst, and besides I'm not set up to do reactions under nitrogen gas, a lot of equipment is involved in that one.

[borohydride]

^That yield has since been debunked. They didn't seem to notice that the -O- bridge had been broken. Later papers cite 65% yield, as does the patent.

I think you will find that the N2 blanket isn't needed. They so often cite a protective atmosphere when it isn't needed. I can see several places selling 1g of RuCl3 for about £40 + P&P. It isn't quite as simple, but the yield is quite a lot higher!