HRID1814099
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
PROCEDURE
实验过程
To a mixture of the compound obtained in Example 22 (4) (0.23 g) and tetrahydrofuran (7 ml), triethylamine (0.19 ml) and ethyl chlorocarbonate (0.1 ml) were added at 0° C. and the mixture was stirred at the same temperature for 20 minutes. An ammonia gas was blown into the mixture at 0° C. and the mixture was stirred at the same temperature for 30 minutes. Water was added thereto and the mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The resulting residue was recrystallized (ethyl acetate) to obtain 0.06 g of the desired product as a white crystal.
WORKUP
后处理
- additionwere added at 0° C.
- customwas blown into the mixture at 0° C.
- stirringthe mixture was stirred at the same temperature for 30 minutes
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe resulting residue was recrystallized (ethyl acetate)