HRID231109

反应详情

EQUATION

反应方程式

HRID 231109 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.6 g of 4,5-dichloro-6-methylpyrimidine was dissolved in 50 ml of toluene. 1.0 g of triethylamine and 2.2 g of 2-[4-(2-ethoxyethyl)-2-methylphenoxy]ethylamine were added to the solution, and the reaction mixture was heated under reflux for 5 hours, whilst stirring. At the end of this time, the reaction mixture was washed with water and dried over anhydrous sodium sulfate. The toluene was removed by distillation under reduced pressure, and the oily product thus obtained was subjected to column chromatography (Wakogel C-200, eluted with a 2:1 by volume mixture of toluene and ethyl acetate) to isolate the product. The crystals thus obtained were recrystallized from hexane to afford 2.6 g of the title compound as colorless needles melting at 57°-58° C.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 5 hours
  3. washAt the end of this time, the reaction mixture was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe toluene was removed by distillation under reduced pressure
  6. customthe oily product thus obtained
  7. washeluted with a 2:1 by volume mixture of toluene and ethyl acetate)
  8. customto isolate the product
  9. customThe crystals thus obtained
  10. customwere recrystallized from hexane