反应详情

A solution of 4-(4-amino-3-fluorobenzoyl)-1-(4-(1,1,1,3,3,3-hexafluoro-2-hydroxypropan-2-yl)benzyl)piperazin-2-one (0.405 mmol, 200 mg) and 4-nitrophenyl carbonochloridate (0.405 mmol, 82 mg) in 1,4-dioxane (2 mL) was stirred at room temperature for 30 minutes. Cyclopropylmethanamine (0.405 mmol, 28.8 mg) and triethylamine (1.216 mmol, 123 mg) were added and the reaction stirred at room temperature overnight. The reaction mixture was diluted with dichloromethane (10 mL) and washed with saturated aqueous sodium hydrogen carbonate solution (10 mL). The organic phase was concentrated and the resulting residue was purified by column chromatography on silica gel (eliciting with 3% methanol/97% dichloromethane—10% methanol/90% dichloromethane gradient) to afford the title compound (45 mg).

1. washwashed with saturated aqueous sodium hydrogen carbonate solution (10 mL)
2. concentrationThe organic phase was concentrated
3. customthe resulting residue was purified by column chromatography on silica gel (eliciting with 3% methanol/97% dichloromethane—10% methanol/90% dichloromethane gradient)