HRID1458731
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) is heated at 80° C. overnight. The reaction mixture is poured into water (1 L), and the precipitate that forms is collected by filtration and washed with water. The solid is dissolved in hot ethyl acetate, and then the solution is dried over MgSO4, filtered and evaporated to a small volume. Hexane is added, and then the mixture is cooled in an ice bath, and then the product that crystallizes is 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
- filtrationthe precipitate that forms is collected by filtration
- washwashed with water
- dissolutionThe solid is dissolved in hot ethyl acetate
- dry with materialthe solution is dried over MgSO4
- filtrationfiltered
- customevaporated to a small volume
- additionHexane is added
- temperaturethe mixture is cooled in an ice bath
- customthe product that crystallizes
- filtrationis collected by filtration
- washwashed with hexane
- customdried