HRID1156769

反应详情

EQUATION

反应方程式

HRID 1156769 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5 g of 4-carbamoyl-4-piperidino-piperidine, 0.5 g of 5% palladium-on-charcoal catalyst and 50 ml of water is boiled under reflux for 50 hours. The reaction mixture is then cooled, and the catalyst is removed by filtration. The filtrate is concentrated and allowed to stand. The precipitated crystals are collected by filtration, dried and recrystallized from chloroform to give 1,2,3,5,6,7,8,8a-octahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine as colorless crystals, m.p. 193° C. 2,3,5,6,7,8-Hexahydro-2-oxo-imidazo[1,2-a]pyridine-3-spiro-4'-piperidine is obtained from the mother liquor. Overall yield is 65%.

WORKUP

后处理

  1. temperatureunder reflux for 50 hours
  2. temperatureThe reaction mixture is then cooled
  3. customthe catalyst is removed by filtration
  4. concentrationThe filtrate is concentrated
  5. filtrationThe precipitated crystals are collected by filtration
  6. customdried
  7. customrecrystallized from chloroform