HRID1580847

反应详情

EQUATION

反应方程式

HRID 1580847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

34.0 g (0.1 mol) of diphenyl-4,5,6-trichloropyrimid-2-yl-chloromethane in 250 ml of absolute acetonitrile are stirred with 13.6 g (0.2 mol) of imidazole for 3 hours at room temperature and thereafter heated to the boil for 15 minutes. The mixture is then concentrated and the dark brown residue is washed with water and taken up in methylene chloride. After drying with sodium sulphate, treating with active charcoal and filtering, the solution is concentrated. The residue is extracted by boiling with petroleum ether, and the mixture is filtered and again concentrated. Finally, the material is recrystallised from a little acetonitrile. 17.0 g (40% of theory) of the compound of formula ##SPC9##

WORKUP

后处理

  1. temperatureheated to the boil for 15 minutes
  2. concentrationThe mixture is then concentrated
  3. washthe dark brown residue is washed with water
  4. dry with materialAfter drying with sodium sulphate
  5. additiontreating with active charcoal
  6. filtrationfiltering
  7. concentrationthe solution is concentrated
  8. extractionThe residue is extracted
  9. filtrationthe mixture is filtered
  10. concentrationagain concentrated
  11. customFinally, the material is recrystallised from a little acetonitrile