HRID223453

反应详情

EQUATION

反应方程式

HRID 223453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,5-dichloropyrazine (14.9 g, 0.1 mol), piperazine (50.5 g, 0.59 mol), acetone (22.5 ml), water (20 ml) and concentrated aqueous HCl (1.8 ml) was heated at reflux for 3 hr. The reaction mixture was cooled, diluted with water, filtered and the acetone was removed by distillation. The aqueous solution was then extracted thrice with chloroform. The combined extracts were washed twice with water, dried (Na2SO4) and evaporated to dryness to afford 7.3 g of solid, m.p. 98°-102°. J. K. Boissier et al., J. Med. Chem., 6, 541 (1963) report a m.p. of 101° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 hr
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. customthe acetone was removed by distillation
  6. extractionThe aqueous solution was then extracted thrice with chloroform
  7. washThe combined extracts were washed twice with water
  8. dry with materialdried (Na2SO4)
  9. customevaporated to dryness