反应详情

A solution of dimethylsulphoxide (369 mg) in dry dichloromethane (3 ml) was added to a stirred solution of oxalyl chloride (300 mg) in dry dichloromethane (7 ml) at -60° under nitrogen and the resulting solution was stirred at -60° to -64° for 30 minutes. The product of stage (i) (774 mg) in dry dichloromethane (5 ml) was added dropwise and the reaction mixture was stirred between -60° to -63° for 2.5 h. Triethylamine (995 mg) was added and the mixture was allowed to warm to -20°, and quenched with water (15 ml). The layers were separated and the aqueous phase was further extracted with dichloromethane (2×15 ml). The combined organic extracts were dried and evaporated to give the title compound as an oil (830 mg).

1. stirringthe reaction mixture was stirred between -60° to -63° for 2.5 h
2. temperatureto warm to -20°
3. customquenched with water (15 ml)
4. customThe layers were separated
5. extractionthe aqueous phase was further extracted with dichloromethane (2×15 ml)
6. customThe combined organic extracts were dried
7. customevaporated