Plurichemie Anstalt

Indira Ghatak

William Heggie

Philip R Page

Ivan Villax

Michael B Hursthouse

A process for the preparation of .mu.-3-carbopentazane-N.sup.1, N.sup.4 :N.sup.2, N.sup.5 -bis-[bis(triphenylphosphine)rhodium (I)] dinitrate by the reaction of tris(triphenylphosphine)nitratorhodium (I) with hydrazine in degassed methanol under an inert atmosphere.

Process for the preparation of a rhodium complex

The present invention refers to complexes prepared by reacting rhodium trinitrate with a suitable hydrazine and a suitable tertiary phosphine, more specifically to the compounds di(.mu.-hydrazine-N.sup.1 :N.sup.2)-bis[bis(triphenylphosphine)rhodium (I)]dinitrate and .mu.-3-carbopentazane-N.sup.1, N.sup.4 :N.sup.2, N.sup.5 -bis[bis(triphenylphosphine)rhodium (I)]dinitrate, which are homogenous hydrogenation catalysts and their application in the hydrogenation of the exocyclic methylene group of acid addition salts of 6-demethyl-6-deoxy-6-methylene-5-hydroxytetracycline (methacycline) to prepare .alpha.-6-deoxy-5-hydroxy-tetracycline (doxycycline).

Process of preparation of novel rhodium hydrogenation catalysts

The present invention refers to complexes prepared by reacting rhodium trinitrate with a suitable hydrazine and a suitable tertiary phosphine, more specifically to the compounds di(.mu.-hydrazine-N.sup.1 :N.sup.2)-bis[bis(triphenylphosphine)rhodium (I)]dinitrate and .mu.-3-carbopentazane-N.sup.1,N.sup.4 :N.sup.2,N.sup.5 -bis[bis(triphenylphosphine)rhodium (I)]dinitrate, which are homogeneous hydrogenation catalysts and their application in the hydrogenation of the exocyclic methylene group of acid addition salts of 6-demethyl-6-deoxy-6-methylene-5-hydroxytetracycline (methacycline) to prepare .alpha.-6-deoxy-5-hydroxy-tetracycline (doxycycline).

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Indira Ghatak