HRID1456015

反应详情

EQUATION

反应方程式

HRID 1456015 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) 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 fitration, 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. customthe precipitate which formed
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. dissolutionThe solid was dissolved in hot ethyl acetate
  5. dry with materialthe solution was dried over MgSO4
  6. filtrationfiltered
  7. customevaporated to a small volume
  8. additionHexane was added
  9. temperaturethe mixture was cooled in an ice-bath
  10. customthe product which crystallized
  11. customwas collected by fitration
  12. washwashed with hexane
  13. customdried