HRID2267125

反应详情

EQUATION

反应方程式

HRID 2267125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Chlorophenylhydrazine hydrochloride (1.0 g) suspended in 6.0 ml of diethyl ether was dropped into 5 ml of concentrated hydrochloric acid cooled at 0° C. After the reaction solution was stirred for 10 minutes, 462 mg of sodium nitrite dissolved in 2.0 ml of water was dropped into the reaction solution and the mixture was stirred for 2 hours together with raising the temperature up to room temperature. Water was added to the reaction solution, the mixture was extracted with ethyl acetate and the ethyl acetate layer washed with a saturated aqueous saline solution and dried over sodium sulfate. The solvent was evaporated in vacuo to give 506 mg of the title compound as a red oily crude product.

WORKUP

后处理

  1. additionwas dropped into the reaction solution
  2. stirringthe mixture was stirred for 2 hours together
  3. temperaturewith raising the temperature up to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. washthe ethyl acetate layer washed with a saturated aqueous saline solution
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated in vacuo