Reaktion #95219

Reaktionsgleichung

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

3,5-dinitrobenzoyl chloride

→

pure product

Ausbeute 85.0%

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

Ausbeute 85.0%

Lösungsmittel

toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe crude product precipitated from the reaction mixture
2. 2
   FiltrationAfter isolation by filtration
3. 3
   Waschenthe residue was washed with hot petroleum ether
4. 4
   Sonstigefinally recrystallized from methylene chloride

Vorschrift

A solution of 10.9 g (0.05 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole and 12.6 g (0.055 mole) 3,5-dinitrobenzoyl chloride in 200 ml toluene was refluxed for 20 hours. The crude product precipitated from the reaction mixture upon cooling to -10° C. After isolation by filtration, the residue was washed with hot petroleum ether and finally recrystallized from methylene chloride to give 17.5 g (85% yield) of pure product; m.p. 197° C.

Quelle