HRID2165854

反应详情

EQUATION

反应方程式

HRID 2165854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 16.4 g of 3-bromo-7-chloro-N-[1-hydroxycyclohexylmethyl]-4-quinolinamine in 176 ml of dimethylformamide was stirred at room temperature and to it was added 7.54 g of potassium tert-butoxide. The mixture was heated at 130°-140° C. for twenty hours. The reaction mixture was then cooled to room temperature, quenched with water, and extracted with an ether/ethyl acetate solution. Evaporation of solvents resulted in a crude oil which was purified by HPLC using 2:1 hexane/ethyl acetate as the eluent. A solid resulted which was recrystallized from isopropanol to yield 4 g of crystalline solid with a melting point of 216°-218° C.

WORKUP

后处理

  1. temperatureThe mixture was heated at 130°-140° C. for twenty hours
  2. customquenched with water
  3. extractionextracted with an ether/ethyl acetate solution
  4. customEvaporation of solvents
  5. customresulted in a crude oil which
  6. customwas purified by HPLC
  7. customA solid resulted which
  8. customwas recrystallized from isopropanol