1-Chloroethyl chloroformate → 4,4-Difluoropiperidine hydrochloride

Participants

Reaction Steps

In an argon atmosphere, 1-chloroethyl chloroformate (2.62 mL) was added dropwise to the above-obtained N-benzyl-4,4-difluoropiperidine (4.66 g) in methylene chloride (93 mL) at 0° C., and the resultant mixture was stirred at 55° C. for 2 hours, and then cooled in air. The reaction solvent was removed under reduced pressure, and the residue in methanol (93 mL) was refluxed under heat for 4 hours, and then cooled in air. The reaction solvent was removed under reduced pressure, to thereby give the title compound as a solid (3.03 g, 87%).

Provenance & Evidence