反应详情

温度

0 °C

15 mg (0.39 mmol, content 60%) of sodium hydride were added to a solution of 34 mg (0.23 mmol) of quinazolin-4(3H)-one in 5 ml of DMF, and the mixture was stirred under an atmosphere of argon at 0° C. for 30 min. 100 mg (0.19 mmol) of tert-butyl 3-[3-({[4-(bromomethyl)phenyl](cyclopentyl)acetyl}amino)-2-methylphenyl]propanoate, dissolved in 1 ml of DMF, were then added to the reaction solution, and the latter was slowly warmed to toom temperature. After the reaction had gone to completion (monitored by TLC; cyclohexane/ethyl acetate 2:1), 1 ml of saturated ammonium chloride solution was added and the reaction mixture was purified directly by preparative HPLC. This gave 28 mg (0.05 mmol, 25% of theory) of the racemic title compound.

1. additionwere then added to the reaction solution
2. temperaturethe latter was slowly warmed
3. additionwas added
4. customthe reaction mixture was purified directly by preparative HPLC