HRID1485112

反应详情

EQUATION

反应方程式

HRID 1485112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-oxocyclobutanecarboxylic acid (13.5 g) in tetrahydrofuran (135 mL), 1,1′-carbonyldiimidazole (23.0 g) was added under cooling with ice. The mixture was brought to room temperature and stirred for 90 minutes. Benzylamine (15.5 mL) was added and the mixture was stirred at that temperature for 14 hours. The crude product was adsorbed on diatomaceous earth with the solvent being distilled off under reduced pressure. The crude product adsorbed on the diatomaceous earth was purified by silica gel column chromatography (chloroform:methanol=100:0-95:5) to give N-benzyl-3-oxocyclobutanecarboxamide as a colorless solid (16.9 g).

WORKUP

后处理

  1. temperatureunder cooling with ice
  2. customwas brought to room temperature
  3. stirringthe mixture was stirred at that temperature for 14 hours
  4. distillationbeing distilled off under reduced pressure
  5. customwas purified by silica gel column chromatography (chloroform:methanol=100:0-95:5)