Preparation of 9.alpha.-fluoro-16.alpha.-methyl-21-acetoxy-.DELT

Details Preparation of 9.alpha.-fluoro-16.alpha.-methyl-21-acetoxy-.DELT Preparation of 9.alpha.-fluoro-16.alpha.-methyl-21-acetoxy-.DELT

1979-11-16

1981-07-07

Roberts, Elbert L.

Chemistry of carbon compounds

Miscellaneous organic carbon compounds

C-metal

C07J 500

Patent

active

042774098

ABSTRACT:
An improved process for the preparation of pure 9.alpha.-fluoro-16.alpha.-methyl-21-acetoxy-.DELTA..sup.1,4 -pregnadiene-11.beta.-ol-3,20-dione comprising reacting 9.alpha.-fluoro-21-acetoxy-.DELTA..sup.1,4,16 -pregnatriene-11.beta.-ol-3,20-dione with a methyl magnesium halide in the presence of a catalytic amount of a cuprous halide effecting protonation of magnesian to form 9.alpha.-fluoro-16.alpha.-methyl-21-acetoxy-.DELTA..sup.1,4 -pregnadiene-11.beta.-ol-3,20-dione, reacting the raw product with an acetylation agent to acetylate the partially deacetylated product and purifying the reacetylated product with an organic solvent, treating in solution with a peroxidation agent and then purifying again with an organic solvent.

REFERENCES:
patent: 3081297 (1963-03-01), Wettstein et al.
patent: 3251866 (1966-05-01), Lincoln et al.
patent: 3312692 (1967-04-01), Oliveto et al.
patent: 3375261 (1968-03-01), Arth et al.

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