HRID1013915

反应详情

EQUATION

反应方程式

HRID 1013915 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.17 g (0.0149 moles) of the N-(4-chloro-3-cyano-7-ethoxy-6-quinolinyl)acetamide, 4.04 g (0.0173 moles) of 4-benzyloxy-3-chloro-phenylamine (example 5), and 2.0 g (0.017 moles) of pyridine hydrochloride in 85 ml of isopropanol was stirred and refluxed in an oil bath for 30 minutes. The reaction was cooled in an ice bath, and the solid was collected by filtration and washed with isopropanol, and then with ether yielding 7.26 g of crude product as the hydrochloride salt. This material was purified by chromatography of the free base on silica gel by elution with 1:39 methanol-methylene chloride.

WORKUP

后处理

  1. temperaturerefluxed in an oil bath for 30 minutes
  2. temperatureThe reaction was cooled in an ice bath
  3. filtrationthe solid was collected by filtration
  4. washwashed with isopropanol
  5. customThis material was purified by chromatography of the free base on silica gel by elution with 1:39 methanol-methylene chloride