HRID395672

反应详情

EQUATION

反应方程式

HRID 395672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 ml) was stirred with heating under reflux for 16 hours. The reaction mixture was concentrated and poured into water (1 L). The solid precipitates were filtered, washed with water and then isopropyl ether, and air-dried. The residue was dried under reduced pressure to give crystals of 2-hydroxy-3′,4′-dichloroacetophenone (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale yellow prisms. Melting point 115-118° C.

WORKUP

后处理

  1. temperaturewith heating
  2. temperatureunder reflux for 16 hours
  3. concentrationThe reaction mixture was concentrated
  4. additionpoured into water (1 L)
  5. customThe solid precipitates
  6. filtrationwere filtered
  7. washwashed with water
  8. dry with materialisopropyl ether, and air-dried
  9. customThe residue was dried under reduced pressure