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
- 70 °C
PROCEDURE
实验过程
1-(t-Butylamino)-N-(2-methyl-5-(3-(trifluoromethyl)benzamido)phenyl)isoquinoline-5-carboxamide (0.13 g, 0.25 mmol) obtained in Step (3) above was dissolved in tetrahydrofuran (1 mL), slowly added with TFA (3 mL) at 0° C., and stirred for about 4 hours at 70° C. The reaction mixture was cooled to room temperature, and adjusted to have a pH value in a range of 10˜11 by adding a saturated aqueous sodium bicarbonate solution. The reaction mixture was diluted with ethyl acetate, followed by washing with distilled water. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The concentrated compound was purified using silica gel chromatography to obtain the title compound (10 mg, 8%).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- washby washing with distilled water
- customThe organic layer thus obtained
- dry with materialwas dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customThe concentrated compound was purified