HRID1164310

反应详情

EQUATION

反应方程式

HRID 1164310 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

276 mg. of lithium hydride (98%), 40 ml. of benzene and 4.2 g. of 2-methoxypyrroline are boiled at reflux for 2 hours under nitrogen and while stirring well. After cooling to 25° C., 6.6 g. of p-methoxybenzoyl chloride dissolved in 25 ml. of benzene are added and the resulting mixture is stirred under reflux for 2 hours and at room temperature for 16 hours. 100 ml. of ethyl acetate followed by 3.0 g. of lithium hydroxide (98%) dissolved in 25 ml. of water are added to the mixture at room temperature within 15 minutes. The organic phase is washed neutral with water, dried over sodium sulfate and evaporated under reduced pressure. After recrystallization from ethanol, there is obtained 1-(p-methoxybenzoyl)-2-pyrrolidinone having a melting point of 119°-120° C.

WORKUP

后处理

  1. temperatureat reflux for 2 hours under nitrogen
  2. stirringthe resulting mixture is stirred
  3. temperatureunder reflux for 2 hours and at room temperature for 16 hours
  4. washThe organic phase is washed neutral with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customAfter recrystallization from ethanol