Reaktion #95217

Reaktionsgleichung

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

3-nitrobenzoyl chloride

→

pure product

Ausbeute 69.1%

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

Ausbeute 69.1%

Lösungsmittel

xylene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 20 hours
2. 2
   SonstigeUnreacted starting amino compound was recovered
3. 3
   Temperaturby cooling the reaction mixture
4. 4
   Filtrationfiltering the resulting precipitate
5. 5
   EinengenThe filtrate was concentrated in vacuo
6. 6
   Sonstigethe residue recrystallized from xylene
7. 7
   WaschenAfter washing with petroleum ether

Vorschrift

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.

Quelle