HRID1640068

反应详情

EQUATION

反应方程式

HRID 1640068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A solution of 5.01 g (30.0 mmol) of 2-acetoxy-6-hydroxytoluene in 50 mL of acetonitrile was added with 12.44 g (90.0 mmol) of potassium carbonate and 12.77 g (90.0 mmol) of methyl iodide and heated and stirred on a 90° C. oil bath for 96 minutes. The reaction mixture which had been allowed to stand at room temperature for about 3 hours was added to a mixture of 100 mL of toluene and 100 mL of water stirred on an ice-water bath, and after stirred for two minutes, transferred to a separatory funnel and then settled. The aqueous layer was separated and discarded and after the organic layer was washed with 20 mL of 1 N aqueous sodium hydroxide and 20 mL of water three times, and the solvent was evaporated to obtain 4.69 g of title compound.

WORKUP

后处理

  1. temperatureheated
  2. waitto stand at room temperature for about 3 hours
  3. stirringstirred on an ice-water bath
  4. stirringafter stirred for two minutes
  5. customtransferred to a separatory funnel
  6. customThe aqueous layer was separated
  7. washafter the organic layer was washed with 20 mL of 1 N aqueous sodium hydroxide and 20 mL of water three times
  8. customthe solvent was evaporated