HRID1410291

反应详情

EQUATION

反应方程式

HRID 1410291 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 5-bromo-2-chloro-4-methoxybenzonitrile (3, 30.6 g, 124 mmol) in ethanol (450 mL)/H2O (225 mL) was added sodium hydroxide (124 g, 3.1 mol). The solution was refluxed at 100° C. overnight, cooled to room temperature and evaporated to remove ethanol. The aqueous layer was cooled to 0° C., acidified with concentrated hydrogen chloride (190 mL). The generated white solid was filtered, washed with water and dried in vacuo to yield the title compound (32 g, 122 mmol, 98%) as a white solid.

WORKUP

后处理

  1. temperaturecooled to room temperature
  2. customevaporated
  3. customto remove ethanol
  4. temperatureThe aqueous layer was cooled to 0° C.
  5. filtrationThe generated white solid was filtered
  6. washwashed with water
  7. customdried in vacuo