HRID1861933
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 (152 mg) obtained in Example 179, methanol (10 ml) and chloroform (10 ml), hydrazine monohydrate (0.05 ml) was added and heated under reflux for 24 h. The reaction mixture was filtered and the filtrate was concentrated under reduced pressure; following addition of 2 N HCl, the mixture was washed with ethyl acetate. Then, the aqueous layer was made alkaline with a 2 N aqueous sodium hydroxide solution and extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure to give 71 mg of the titled compound (yield, 78%).
WORKUP
后处理
- additionwas added
- temperatureheated
- temperatureunder reflux for 24 h
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated under reduced pressure
- additionaddition of 2 N HCl
- washthe mixture was washed with ethyl acetate
- extractionextracted with ethyl acetate
- washThe organic layer was washed with a saturated aqueous sodium chloride solution
- dry with materialdried with anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure