Methyl chloroformate → HCID 15020371, compound

Participants

Reaction Steps

A mixture of α,α-bis(4-fluorophenyl)-4-piperidineacetamide (7.65 g, 0.023 mol) and sodium bicarbonate (3.36 g, 0.023 mole) in methylene chloride was prepared. To this mixture was added a solution of methyl chloroformate (2.17 g, 0.023 mole) in methylene chloride. The resulting mixture was stirred overnight at room temperature. The mixture was extracted successively with water, 5% sodium hydroxide, and water. The methylene chloride layer was dried (sodium sulfate). The organic layer was filtered, and solvent was removed to provide a fluffy, white residue (5.95 g, 66.6% yield). A 0.5 g sample was crystallized from methylene chloridehexanes. This provided a white solid which was dried in vacuo overnight at 80° C., mp 126°-129° C.

Provenance & Evidence