HRID1458661

反应详情

EQUATION

反应方程式

HRID 1458661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

58.6 g (0.39 mol) of 4,6-dichloropyrimidine were placed in 400 ml of toluene, and a mixture of 61.0 g (0.39 mol) of cis-4-tert-butylcyclohexylamine and 50.0 g (0.50 mol) of triethylamine in 100 ml of toluene was added dropwise at from 70° to 80° C. The mixture was subsequently stirred at reflux for 4 hours. After cooling, it was extracted by stirring with water, the organic phase was dried and concentrated, to give a colorless oil which crystallized after trituration with petroleum ether. Filtration with suction left 70.5 g (67.0% of theory) of colorless crystals.

WORKUP

后处理

  1. additionwas added dropwise at from 70° to 80° C
  2. temperatureat reflux for 4 hours
  3. temperatureAfter cooling
  4. extractionit was extracted
  5. stirringby stirring with water
  6. customthe organic phase was dried
  7. concentrationconcentrated
  8. customto give a colorless oil which
  9. customcrystallized after trituration with petroleum ether
  10. filtrationFiltration with suction
  11. waitleft 70.5 g (67.0% of theory) of colorless crystals