HRID1038381

反应详情

EQUATION

反应方程式

HRID 1038381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 9.5 g (34.1 mmol) 4-(3-cyano-4-fluorophenyl)-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarbonitrile (Example 1A) and 10 g (312 mmol) hydrazine hydrate in n-butyl alcohol (75 ml) was stirred at 80° C. for 5 h. The mixture was cooled and concentrated under reduced pressure. Saturated aqueous sodium bicarbonate solution was added to the residue, and the mixture was extracted with ethyl acetate. The organic phases were combined, dried over sodium sulfate, and concentrated under reduced pressure to afford the title compound (5.6 g, 57% of th.) as a pale yellow solid.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. concentrationconcentrated under reduced pressure
  3. additionSaturated aqueous sodium bicarbonate solution was added to the residue
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure