HRID596999

反应详情

EQUATION

反应方程式

HRID 596999 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

A stirred mixture of 2,3-dichloroanisole (100 g., 0.565 mole) and isobutyryl chloride (66 g., 0.62 mole) in methylene chloride (400 ml.) is cooled to 5° C. and treated with aluminum chloride (83 g., 0.62 mole) during a 1 -hour period. The reaction mixture is allowed to warm to 25° C. and after 24 hours is poured into ice water (400 ml.) and hydrochloric acid (30 ml.). The organic phase is washed with 5% sodium hydroxide, water, dried over magnesium sulfate and distilled at reduced pressure affording 68 g. of 2',3'-dichloro-4'-methoxyisobutyrophenone which distills at 120°-130° C./0.5 mm.

WORKUP

后处理

  1. temperatureto warm to 25° C. and after 24 hours
  2. washThe organic phase is washed with 5% sodium hydroxide, water
  3. dry with materialdried over magnesium sulfate
  4. distillationdistilled at reduced pressure
  5. customaffording 68 g
  6. distillationof 2',3'-dichloro-4'-methoxyisobutyrophenone which distills at 120°-130° C./0.5 mm