反应详情

To a stirred solution of bis(trichloromethyl) carbonate (0.076 mmol, 22.60 mg) in dichloromethane (3 mL) was added triethylamine (40 mL) and 3-((4-(4-amino-2-chloro-3-fluorobenzoyl)piperazin-1-yl)methyl)-N-tert-butylbenzamide (0.206 mmol, 92 mg) in dichloromethane (3 mL). The reaction mixture was heated to reflux for 2 hours. After this time the reaction was allowed to cool to room temperature and cyclopropylmethylamine (35 μl, 0.412 mmol) and triethylamine (35 μl) were added. After 30 minutes stirring, the volatiles were removed under reduced pressure and the crude residue was purified by silica chromatography (eluting with 5% methanol in dichloromethane) to yield the title compound (80 mg).

1. temperatureThe reaction mixture was heated
2. temperatureto reflux for 2 hours
3. customthe volatiles were removed under reduced pressure
4. customthe crude residue was purified by silica chromatography (eluting with 5% methanol in dichloromethane)