Methyl chloroformate → HCID 15645978, compound

Participants

Reaction Steps

A solution of methylchloroformate (243 mg) in dry dichloromethane (3 ml) was added dropwise to a stirred solution of 1-[(3,4-dichlorophenyl)acetyl]-2-[(3-hydroxy-1-pyrrolidinyl)methyl]piperazine dihydrochloride (1.0 g) and triethylamine (495 mg) in dry dichloromethane (25 ml) at -25° under nitrogen. The resulting solution was stirred at -30°--25° for 30 min, quenched with aqueous 2N sodium carbonate solution (30 ml) and extracted with dichloromethane (3×20 ml). The combined organic extracts were dried and evaporated to give a foam. The residue was purified by flash column chromatography eluting with dichloromethane:methanol:0.880 NH3 (150:8:1) to give the title compound as a foam (800 mg).

Provenance & Evidence