Реакция #95217

Уравнение реакции

5-amino-3-trichloromethyl-1,2,4-thiadiazole

3-nitrobenzoyl chloride

→

pure product

Выход 69.1%

5-(3-Nitrobenzamido)-3-Trichloromethyl-1,2,4-Thiadiazole

Выход 69.1%

Растворители

xylene

Условия реакции

Обработка

1. 1
   Температураat reflux for 20 hours
2. 2
   ДругоеUnreacted starting amino compound was recovered
3. 3
   Температураby cooling the reaction mixture
4. 4
   Фильтрацияfiltering the resulting precipitate
5. 5
   КонцентрированиеThe filtrate was concentrated in vacuo
6. 6
   Другоеthe residue recrystallized from xylene
7. 7
   ПромывкаAfter washing with petroleum ether

Методика

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.

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