HRID977123
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 1-ethyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (11.6 g, 0.05 mol), DMSO (20 ml) and phenethylamine (12.1 g, 0.1 mol) was heated at 80° C. overnight. The reaction mixture was poured into water (1 L) and the precipitate which formed was collected by filtration and washed with water. The solid was dissolved in hot ethyl acetate, and then the solution was dried over MgSO4, filtered and evaporated to a small volume. Hexane was added and then the mixture was cooled in an ice-bath and then the product which crystallized was collected by filtration, washed with hexane and dried to afford 12.5 g of 1-ethyl-N-(phenylethyl)-1H-pyrazolo[3,4-b]quinoline-4 amine, m.p. 157°-158° C.
WORKUP
后处理
- customthe precipitate which formed
- filtrationwas collected by filtration
- washwashed with water
- dissolutionThe solid was dissolved in hot ethyl acetate
- dry with materialthe solution was dried over MgSO4
- filtrationfiltered
- customevaporated to a small volume
- additionHexane was added
- temperaturethe mixture was cooled in an ice-bath
- customthe product which crystallized
- filtrationwas collected by filtration
- washwashed with hexane
- customdried