HRID2050084

反应详情

EQUATION

反应方程式

HRID 2050084 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

A solution of sodium hydroxide (50%, 300 ml) is added to a solution of p-methoxyphenylacetonitrile (147 g, 1 mol), dicyclohexyl-18-crown-6 (18.63 g, 5 mol %), 2-bromopropane (320 g, 2.6 mol) and benzene (300 ml). The reaction mixture is heated to 45° C. and held for 4 days. The organic phase is separated, washed well with water (3×200 ml), dilute hydrochloric acid (1×200 ml), water (2×200 ml) and evaporated to an oil. Vacuum distillation gives the product (175.6 g, 81% real): boiling point 96° C. to 100° C. (0.15 mm); nmr (CDCl3) shows that the distilled material contains 12.5 mol % of the starting nitrile.

WORKUP

后处理

  1. customThe organic phase is separated
  2. washwashed well with water (3×200 ml), dilute hydrochloric acid (1×200 ml), water (2×200 ml)
  3. customevaporated to an oil
  4. distillationVacuum distillation
  5. customgives the product (175.6 g, 81% real)