Methyl chloroformate → HCID 70674229, compound

Participants

Reaction Conditions

Reaction Steps

1.84 g (4.642 mmol) of the compound prepared in Example 9A were initially charged in pyridine (35 ml), 0.359 ml (4.642 mmol) of methyl chloroformate was added at 0° C. and the mixture was stirred at 0° C. for 10 min. After 16 hours of stirring at 20° C., the reaction mixture was poured into ice-water and extracted three times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride solution, dried over sodium sulfate, filtered and concentrated. The residue was purified by chromatography on silica gel (mobile phase:gradient dichloromethane:methanol 100:5 to dichloromethane:methanol 2:1). This gave 1.13 g of the target compound (53% of theory).

Provenance & Evidence