HRID236913

反应详情

EQUATION

反应方程式

HRID 236913 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

126 g (1 mol) of dimethylmaleic anhydride and 115 g (1 mol) of 4-aminocyclohexanol are warmed, in an oil bath whilst stirring, to 120° to 125° C. (internal temperature) for 30 minutes. After cooling to 20° C., the reaction product is dissolved in 500 ml of methylene chloride and extracted once with 100 ml of 1 NaOH, whilst cooling with ice. The reaction product is then washed twice with water and dried over sodium sulphate. The solvent is evaporated and the residue is recrystallised from a 1:1 mixture by volume of ethyl acetate and petroleum ether. 155 g (70% of theory) of N-(4-hydroxycyclohexyl)-dimethylmaleimide are obtained; melting point 109° to 111° C.

WORKUP

后处理

  1. extractionextracted once with 100 ml of 1 NaOH
  2. temperaturewhilst cooling with ice
  3. washThe reaction product is then washed twice with water
  4. dry with materialdried over sodium sulphate
  5. customThe solvent is evaporated
  6. customthe residue is recrystallised from a 1:1 mixture by volume of ethyl acetate and petroleum ether