HRID1458746

反应详情

EQUATION

反应方程式

HRID 1458746 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1,3-dimethyl-4-chloro-1H-pyrazolo[3,4-b]quinoline (1.2 g, 0.005 mol), benzylamine (1.2 ml) and DMSO (3 ml) is heated at 80°-90° C. for 3-4 hours. The reaction mixture is cooled to room temperature and then is poured into water. The mixture is extracted with CH2Cl2 (3×50 ml) and then the CH2Cl2 layers are combined and evaporated. The residue is purified by column chromatography on silca gel eluting with ethyl acetate to afford the product which is crystallized from ether/hexane to afford 1.2 g of 1,3-dimethyl-N-(phenylmethyl)-1H-pyrazolo[3,4-b]quinolin-4-amine, as a yellow solid, m.p. 105° C.

WORKUP

后处理

  1. temperatureis heated at 80°-90° C. for 3-4 hours
  2. extractionThe mixture is extracted with CH2Cl2 (3×50 ml)
  3. customevaporated
  4. customThe residue is purified by column chromatography on silca gel
  5. washeluting with ethyl acetate
  6. customto afford the product which
  7. customis crystallized from ether/hexane