HRID250280

反应详情

EQUATION

反应方程式

HRID 250280 的结构方程式

CONDITIONS

反应条件

温度
138 °C

PROCEDURE

实验过程

A stirred solution of 2-bromo-6-fluorobenzaldehyde (2.3 Kg, 11.33 moles) and mercaptoacetic acid (1.04 Kg, 11.33 mole) is added to a solution of KOH (951 g, 16.99 mol) in dimethylformamide (11.0 L) at room temperature. The reaction mixture is stirred for 1.5 h at 136 to 140° C. Upon completion of the reaction, the reaction mixture is cooled to 10° C. and quenched with concentrated HCl (2.5 L). The mixture is stirred for 1 h at 10° C. and the resulting solid is filtered. The filtered cake is washed with water (2×3 L) and dried under vacuum to afford the title compound (2.2 Kg, 76%) as a yellow solid.

WORKUP

后处理

  1. customUpon completion of the reaction
  2. temperaturethe reaction mixture is cooled to 10° C.
  3. customquenched with concentrated HCl (2.5 L)
  4. stirringThe mixture is stirred for 1 h at 10° C.
  5. filtrationthe resulting solid is filtered
  6. washThe filtered cake is washed with water (2×3 L)
  7. customdried under vacuum