HRID484070

反应详情

EQUATION

反应方程式

HRID 484070 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

While 2 g of sodium hydride (60% oily) was being stirred in 50 ml of tetrahydrofuran, 5 g of 3-methyl-2-pyrrolidinone was added to the mixture, and the resulting mixture was stirred at room temperature for 1 hour. The reaction mixture was cooled to not higher than 0° C., and 7.5 g of 4-methoxyphenyl isocyanate was added dropwise to the mixture, followed by stirring at the same temperature for 5 hours. Acetic acid was then added to the reaction mixture for neutralization, water was thereafter added to the mixture, and the solvent was distilled off in a vacuum. Water was added to the residue, and the precipitate was filtered off, giving 8.2 g of 3-methyl-1-(4-methoxyphenylcarbamoyl)-2-pyrrolidinone (yield 66%) having a melting point of 71° to 72° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to not higher than 0° C.
  2. stirringby stirring at the same temperature for 5 hours
  3. additionwas thereafter added to the mixture
  4. distillationthe solvent was distilled off in a vacuum
  5. additionWater was added to the residue
  6. filtrationthe precipitate was filtered off