HRID231120

反应详情

EQUATION

反应方程式

HRID 231120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.0 g of 4-{2-[4-(2-bromoethyl)-2-methylphenoxy]ethylamino}-5-chloro-6-methylpyrimidine and 1.4 g of morpholine were dissolved in 40 ml of ethanol, and the mixture was charged into an autoclave. Then, the mixture was allowed to react at 120° to 130° C. for 8 hours. At the end of this time, the ethanol was removed by distillation and water was added to the residue. The oily substance which separated was then extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate, after which the ethyl acetate was removed by distillation under reduced pressure to obtain an oily substance. The substance obtained was subjected to column chromatography (Wakogel C-200, eluted with ethanol), to obtain 2.6 g of the title compound as a pale yellow oily liquid, n25.7 =1.5643.

WORKUP

后处理

  1. additionthe mixture was charged into an autoclave
  2. customto react at 120° to 130° C. for 8 hours
  3. customAt the end of this time, the ethanol was removed by distillation and water
  4. additionwas added to the residue
  5. customThe oily substance which separated
  6. extractionwas then extracted with ethyl acetate
  7. washThe extract was washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. customafter which the ethyl acetate was removed by distillation under reduced pressure
  10. customto obtain an oily substance
  11. customThe substance obtained
  12. washwas subjected to column chromatography (Wakogel C-200, eluted with ethanol)