HRID126928

反应详情

EQUATION

反应方程式

HRID 126928 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 22.6 g (0.20 mole) of 3,4-epoxy-1-ethyl-pyrrolidine, 29.2 g (0.40 mol) of n-butylamine and one drop of conc. hydrochloric acid was heated in a bomb at 150° C. for 20 hr. The mixture was cooled to room temperature, diluted with 350 ml of petroleum ether, cooled in an ice bath and the precipitate was collected. The yield of pure compound as white flakes in this step was 18.0 g (48%); m.p. 57.5°-59.0° C. The filtrate was concentrated under high vaccum leaving a residue of 17.5 g (47%) of quite pure product. Total yield in the two steps was 35.5 g (about 95%).

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. temperaturecooled in an ice bath
  3. customthe precipitate was collected
  4. concentrationThe filtrate was concentrated under high vaccum
  5. customleaving a residue of 17.5 g (47%) of quite pure product
  6. customTotal yield in the two steps