HRID596989

反应详情

EQUATION

反应方程式

HRID 596989 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 75 g. (0.5 m.) of methyl salicylate in 200 ml. of tetrachloroethylene is cooled in an ice bath and treated with a solution of 40 g. (0.5 m.) of acetyl chloride in 200 ml. of tetrachloroethylene. To the chilled mixture is added 133 g. (1.0 m.) of aluminum chloride over a fifteen minute period, maintaining the temperature below 25° C. After the adddition is completed the mixture is stirred for 4 hours at 25° C. and then poured into ice water. The organic layer is separated, washed with water and saturated aqueous sodium bicarbonate solution, dried and evaporated. The residual oil is crystallized from hexane to give methyl 5-acetylsalicylate, m.p. 60°-62° C.

WORKUP

后处理

  1. additiontreated with a solution of 40 g
  2. additionTo the chilled mixture is added 133 g
  3. temperaturemaintaining the temperature below 25° C
  4. customThe organic layer is separated
  5. washwashed with water and saturated aqueous sodium bicarbonate solution
  6. customdried
  7. customevaporated
  8. customThe residual oil is crystallized from hexane