HRID1181497
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 60 °C
PROCEDURE
实验过程
N-[1-(Methoxycarbonyl)isoquinolin-5-yl]-N′-[4-(trifiluoromethyl)benzyl]urea (Example 116, 70 mg, 0.174 mmol) was suspended in a mixture of THF (5 ml) and toluene (5 ml). Lithium borohydride (50 mg, 2.27 mmol) was added and the reaction mixture heated at 60° C. for 1 hour. The reaction was cooled to room temperature and allowed to stand for 1 week. The crystalline product was collected by filtration, washed with toluene (2 ml), then triturated with 1:1 TBF-dichloromethane (2 ml), triturated again with THF (2 ml) and dried under vacuum to give the title compound (8 mg, 12%). m/z (ES+) 376 (M+H)+.
WORKUP
后处理
- temperatureThe reaction was cooled to room temperature
- waitto stand for 1 week
- filtrationThe crystalline product was collected by filtration
- washwashed with toluene (2 ml)
- customtriturated with 1:1 TBF-dichloromethane (2 ml)
- customtriturated again with THF (2 ml)
- customdried under vacuum