HRID1174117
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
A solution of the product of Example 3F (28.44 g, 78.9 mmol) in ethanol (400 mL) was treated with hydrazine hydrate (25 mL, 789 mmol), stirred at 70° C. for 2 hours, cooled to 25° C. The solid precipitate was dissolved by addition of aqueous NaOH solution (200 mL, 1 N). The reaction was partitioned between dichloromethane and water. The aqueous was extracted three times with dichloromethane. The combined organic extracts were dried over MgSO4, filtered and concentrated to give the title compound (15.4 g, 85% yield), which was used without further purification.
WORKUP
后处理
- temperaturecooled to 25° C
- customThe reaction was partitioned between dichloromethane and water
- extractionThe aqueous was extracted three times with dichloromethane
- dry with materialThe combined organic extracts were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated