HRID1844839

反应详情

EQUATION

反应方程式

HRID 1844839 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

In a dried reaction flask, 4-fluoro-2-methylbenzonitrile (4.055 g, 30.0 mmol) and hydrazine hydrate (85%) (3.54 mL, 60.0 mmol) were dissolved in ethanol (15.9 mL). In the protection from light and under the nitrogen atmosphere, the solution was heated under reflux at 80° C. for 48 hr. Water was added to the reaction solution. The mixture was filtered. The filtered cake was rinsed with water to produce a pale yellow solid, which was suspended in ethyl ether. A hydrogen chloride gas was passed into the suspension under an ice-salt bath. The suspension was filtered. The filtered cake was rinsed with ethyl ether to produce an off-white solid (2.04 g) in 37.0% yield.

WORKUP

后处理

  1. temperatureIn the protection from light and under the nitrogen atmosphere, the solution was heated
  2. filtrationThe mixture was filtered
  3. washThe filtered cake was rinsed with water
  4. customto produce a pale yellow solid, which
  5. filtrationThe suspension was filtered
  6. washThe filtered cake was rinsed with ethyl ether