HRID877435
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
A stirred solution of compound 2 (2.1 g, 9.8 mmol) and hydrazine hydrate (2.4 mL, 49.0 mmol) in ethanol (70 mL) was heated to reflux for 8 h. On completion, solvent was removed, diluted with water (30 mL) and extracted with 10% methanol in dichloromethane (60 mL×4). The combined organic layer was washed with brine, dried over sodium sulphate and concentrated to afford the title compound 3 (2.0 g, 91%) which was used for further reaction.
WORKUP
后处理
- temperatureto reflux for 8 h
- customOn completion, solvent was removed
- additiondiluted with water (30 mL)
- extractionextracted with 10% methanol in dichloromethane (60 mL×4)
- washThe combined organic layer was washed with brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated