HRID485690

反应详情

EQUATION

反应方程式

HRID 485690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

4.7 g of pyridine are added to a solution of 7.8 g of 3-methylthio-5-amino-1H-1,2,4-triazole [Monatshefte fur Chemie 106, 1291 (1975)] in 200 ml of dioxane, then 10.8 g of 4-chloro-benzoylchloride are added dropwise at -5° C. The reaction mixture is stirred for one hour at -5° C., then for a further one hour at room temperature, finally 100 ml of water are added at water-cooling and the entire mixture is extracted with chloroform. The chloroform layer is washed with water, dried, evaporated to dryness, yielding 13.46 g (83.5 percent) of 1-(4-chloro-benzoyl)-3-methylthio-5-amino-1,2,4-triazole, m.p. 175° to 177° C. (following boiling with alcohol).

WORKUP

后处理

  1. waitfor a further one hour at room temperature
  2. temperaturecooling
  3. extractionthe entire mixture is extracted with chloroform
  4. washThe chloroform layer is washed with water
  5. customdried
  6. customevaporated to dryness