HRID5816

反应详情

EQUATION

反应方程式

HRID 5816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2-Chloroquinoxaline (2 g) and sodium hydrosulphide (1.23 g) were stirred together in 25 ml of dimethylformamide and heated to 100° C. After 3 hours the reaction mixture was allowed to cool and then partitioned between 70 ml of water and 30 ml of ethyl acetate. The organic layer was separated and the aqueous layer extracted twice with 20 ml of ethyl acetate. The combined organic extracts were washed with sodium chloride solution, dried over anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure to yield an orange solid (3.1 g). The product of this reaction was used in the next preparative step without further purification.

WORKUP

后处理

  1. temperatureto cool
  2. custompartitioned between 70 ml of water and 30 ml of ethyl acetate
  3. customThe organic layer was separated
  4. extractionthe aqueous layer extracted twice with 20 ml of ethyl acetate
  5. washThe combined organic extracts were washed with sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure