HRID1458731

反应详情

EQUATION

反应方程式

HRID 1458731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. filtrationthe precipitate that forms is collected by filtration
  2. washwashed with water
  3. dissolutionThe solid is dissolved in hot ethyl acetate
  4. dry with materialthe solution is dried over MgSO4
  5. filtrationfiltered
  6. customevaporated to a small volume
  7. additionHexane is added
  8. temperaturethe mixture is cooled in an ice bath
  9. customthe product that crystallizes
  10. filtrationis collected by filtration
  11. washwashed with hexane
  12. customdried