HRID329019
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customSome precipitate had formed
- customA solid precipitated which
- filtrationwas filtered off
- washwashed with cold water
- customRecrystallization from 300 ml ethanol