HRID1458729

反应详情

EQUATION

反应方程式

HRID 1458729 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 (15.0 g, 0.065 mol), benzylamine (15.6 ml, 0.14 mol) and DMSO (100 ml) is heated at 80° C. overnight. The reaction mixture is poured into ice/water and the gummy solid which formed is collected by filtration. The solid is dissolved in ethyl acetate, dried over MgSO4, filtered and concentrated. The residual oil is crystallized from ethyl acetate to afford 18 g (92%) of 1-ethyl-N-(phenyl methyl)-1H-pyrazolo[3,4-b]quinolin-4-amine, m.p. 130°-132° C.

WORKUP

后处理

  1. customthe gummy solid which formed
  2. filtrationis collected by filtration
  3. dissolutionThe solid is dissolved in ethyl acetate
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residual oil is crystallized from ethyl acetate