HRID1061853

反应详情

EQUATION

反应方程式

HRID 1061853 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. extractionextracted with ethyl ether
  2. washwashed with HCl (2N)
  3. dry with materialdried over MgSO4
  4. customEvaporation and crystallization from ethyl ether/hexanes