Phosphorus oxychloride → HCID 19764418, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 160 mg of 3,3-difluoro-2-methyl-2-nonadecanol in 2 ml of pyridine containing 50 ul of phosphorous oxychloride is heated at 90° C. then allowed to cool to 50° C. An additional 250 ul of phosphorous oxychloride is added followed by heating at 90° C. for 2 hours. After allowing to stand at ambient temperature for 18 hours, the volatiles are removed and the concentrate partitioned between hexanes and 10% hydrochloric acid. The organic layer is washed with water and 10% sodium bicarbonate then dried and evaporated to a residue which is purified by chromatography on silica gel using hexane to give 140 mg of the desired product as an oil.

Provenance & Evidence