m-Chloroperbenzoic acid → HCID 15057075, compound

Participants

Reaction Steps

To a solution of 2.0 g (7.54 mmol) of 2-oxo-1-[[2-(pyridin-2-ylthio)ethyl]carbamoyl]pyrrolidine in 35 ml of CH2Cl2 was added 1.63 g (7.54 mmol) of m-CPBA (content 80%) under ice-cooling. Then the mixture was stirred for 1.5 hr. at room temperature. The reaction solution was washed with aqueous NaHCO3 and water. After drying, the solvent was removed by evaporation. The residue was refined by silica gel column chromatography, then the crystalline objective compound was obtained from the eluate with benzene/ethyl acetate (3/1-1/1 v/v). The compound was washed with Et2O and collected by filtration, whereby 0.93 g of the crystalline compound (I b-3) melting at 119.5°-120.5° C. was obtained. Yield: 43.9%.

Provenance & Evidence