HRID1164311

反应详情

EQUATION

反应方程式

HRID 1164311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.2 g. of 2-methoxypyrroline are dissolved in 25 ml. of benzene and treated at room temperature with 6.6 g. of p-methoxybenzoyl chloride dissolved in 30 ml. of benzene. The mixture is stirred at room temperature for 60 minutes and at reflux for 4 hours. 30 ml. of benzene are then added and the mixture is boiled at reflux for a further 24 hours. The volatile constituents are distilled off, the residue is taken up in ethanol, the mixture is concentrated, the residue is triturated with diethyl ether, filtered and the filter cake is taken up in ethyl acetate. The ethyl acetate solution is washed with sodium bicarbonate solution and water, dried over sodium sulfate and concentrated. The residue is sublimed in vacuo and there is obtained 1-(p-methoxybenzoyl)-2-pyrrolidinone having a melting point of 119°-120° C.

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. temperatureat reflux for a further 24 hours
  3. distillationThe volatile constituents are distilled off
  4. concentrationthe mixture is concentrated
  5. customthe residue is triturated with diethyl ether
  6. filtrationfiltered
  7. washThe ethyl acetate solution is washed with sodium bicarbonate solution and water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated