HRID2405012

反应详情

EQUATION

反应方程式

HRID 2405012 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
54 °C

PROCEDURE

实验过程

Under argon, 250 g (1.07 mol) of 2-(bromomethyl)-1-fluoro-4-nitrobenzene were introduced as initial charge in 2.5 l of methanol, 371 g (1.60 mol) of silver(I) oxide were added and the mixture was stirred for 2.5 h at 52-56° C. After cooling to RT, suction filtration over kieselguhr was carried out, followed by after-washing with methanol, and the solvent was removed on a rotary evaporator. The crude product was purified by distillation on a short-path evaporator at a jacket temperature of 104° C. and 0.56 mbar. This gave 184.5 g (93%) of the desired product.

WORKUP

后处理

  1. temperatureAfter cooling to RT
  2. filtrationsuction filtration over kieselguhr
  3. washby after-washing with methanol
  4. customthe solvent was removed on a rotary evaporator
  5. distillationThe crude product was purified by distillation on a short-path evaporator at a jacket temperature of 104° C. and 0.56 mbar