Phenyl chloroformate → HCID 20343997, compound

Participants

Reaction Steps

A mixture of 2.5 g of 4-cyano-1-methyl-4-(2-phenylthiophenyl)piperidine, free base of Example 3, and 1.7 g of phenyl chloroformate in 50 ml of methylene chloride is permitted to stand for 24 hours before being poured onto 100 g of ice. Thereafter, the mixture is extracted with 50 ml of methylene chloride and the organic solution is successively washed twice with 50 ml portions of water, washed once with 40 ml saturated sodium bicarbonate solution, washed once with 40 saturated sodium chloride solution, dried and evaporated. The residue is chromatographed through a silica gel column, first with an ether eluant and then with an ether-hexane (1:1) mixture eluant, until there is no indication of contamination by thin layer chromatography. Thereafter, the product is chromatographed through the same absorbent, ether eluant to provide 4-cyano-1-phenoxycarbonyl-4-(2-phenylthiophenyl)piperidine.

Provenance & Evidence