HRID2405012
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling to RT
- filtrationsuction filtration over kieselguhr
- washby after-washing with methanol
- customthe solvent was removed on a rotary evaporator
- distillationThe crude product was purified by distillation on a short-path evaporator at a jacket temperature of 104° C. and 0.56 mbar