HRID1051242
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
- 80 °C
PROCEDURE
实验过程
Methyl 1-(t-butylamino)isoquinoline-5-carboxylate (1.6 g, 6.20 mmol) obtained in Step (5) above was stirred in a solution of tetrahydrofuran (16 mL) and distilled water (16 mL). The reaction solution was added with LiOH (0.57 g, 13.6 mmol) and stirred for about 12 hours at 80° C. The reaction mixture was cooled to room temperature and adjusted to have a pH value in a range of 1˜2 by adding 1N aqueous HCl. The reaction mixture was diluted with ethyl acetate, and washed with distilled water. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to obtain the title compound (0.6 g, 40%).
WORKUP
后处理
- distillationdistilled water (16 mL)
- temperatureThe reaction mixture was cooled to room temperature
- washwashed with distilled water
- customThe organic layer thus obtained
- dry with materialwas dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure