HRID461845

反应详情

EQUATION

反应方程式

HRID 461845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
105 °C

PROCEDURE

实验过程

2-Hydrazinobenzothiazole (125 grams; 0.76 mole), ethyl orthoformate (112.4 grams, 0.76 mole), and 2 liters of xylene were heated together with stirring in a three-necked 5-liter flask. An 8-inch column with a condenser was placed in one neck. The reaction was heated to 105° C. and soon all the solid had gone into solution and the solution turned red. Ethanol began to distill from the reaction and about 125 milliliters of it was collected before the reaction was stopped and allowed to cool to room temperature. The yellow precipitate was collected and triturated with diethyl ether. The s-triazolo(3,4-b)benzothiazole product thus obtained was recrystallized from chloroform, m.p. 174.5°-7° C.

WORKUP

后处理

  1. customAn 8-inch column with a condenser was placed in one neck
  2. distillationto distill from the reaction and about 125 milliliters of it
  3. customwas collected before the reaction
  4. temperatureto cool to room temperature
  5. customThe yellow precipitate was collected
  6. customtriturated with diethyl ether