HRID66939

反应详情

EQUATION

反应方程式

HRID 66939 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 21.8 g (0.1 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 18.6 g (0.1 mole) 3-nitrobenzoyl chloride in 250 ml xylene was heated at reflux for 20 hours. Unreacted starting amino compound was recovered by cooling the reaction mixture and filtering the resulting precipitate. The filtrate was concentrated in vacuo and the residue recrystallized from xylene. After washing with petroleum ether, 25.4 g (69% yield) of pure product was obtained; m.p. 198° C.

WORKUP

后处理

  1. temperatureat reflux for 20 hours
  2. customUnreacted starting amino compound was recovered
  3. temperatureby cooling the reaction mixture
  4. filtrationfiltering the resulting precipitate
  5. concentrationThe filtrate was concentrated in vacuo
  6. customthe residue recrystallized from xylene
  7. washAfter washing with petroleum ether