HRID1061853
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
- 100 °C
PROCEDURE
实验过程
A mixture of (2-fluoro-4-methoxyphenyl)(6-methoxy-2-naphthyl)methanone (1.0 g, 3.22 mmol), 1-methylhydrazine (0.74 g, 16.1 mmol), pyridine (10 mL), and 4-dimethylaminopyridine (0.39 g, 3.22 mmol) was stirred at 100° C. for 12 h. The mixture poured in the water, extracted with ethyl ether, washed with HCl (2N), and dried over MgSO4. Evaporation and crystallization from ethyl ether/hexanes gave an off-white solid (0.82 g, 80% yield, m.p. 166-168° C.); MS m/e 319 (M+H)+.
WORKUP
后处理
- extractionextracted with ethyl ether
- washwashed with HCl (2N)
- dry with materialdried over MgSO4
- customEvaporation and crystallization from ethyl ether/hexanes