HRID329019

反应详情

EQUATION

反应方程式

HRID 329019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Propargyl bromide, 2.38 g, was added to a solution of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine (5.52 g) and triethylamine (3ml) in 90 ml DMF. The reaction mixture was stirred at room temperature for 41/2 hours. Some precipitate had formed. The reaction mixture was poured into 300 ml of cold water. A solid precipitated which was filtered off and washed with cold water. Recrystallization from 300 ml ethanol gave 4.05 g of the title compound as pale yellow needles, m.p. 160°-161.5°. An analytical sample was recrystallized again from ethanol to give almost colorless needles, m.p. 162°-163° C.

WORKUP

后处理

  1. customSome precipitate had formed
  2. customA solid precipitated which
  3. filtrationwas filtered off
  4. washwashed with cold water
  5. customRecrystallization from 300 ml ethanol