Reaktion #347531

Reaktionsgleichung

hydrochloric acid

sodium hydride

3-mercapto-1,2,4-triazole

1-chloro-4-nitrobenzene

→

3-(4-nitrophenylthio)-1,2,4-triazole

Ausbeute 66.0%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGThe solution was stirred at room temperature for one hour
2. 2
   Temperaturrefluxed for 2 hours
3. 3
   Extraktionwas extracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with brine
5. 5
   Trocknendried with magnesium sulfate
6. 6
   Sonstigethe solvent was evaporated
7. 7
   Sonstigeso that coarse crystals were obtained
8. 8
   SonstigeThe coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 7.72 g of the titled compound
9. 9
   Sonstigewas obtained (at a yield of 66%)

Vorschrift

5 g of 3-mercapto-1,2,4-triazole was dissolved in 40 ml of N,N-dimethylformamide, and 2.17 g of sodium hydride (60% in mineral oil) was added at 0° C.. The solution was stirred at the same temperature for one hour, and then 7.78 g of 1-chloro-4-nitrobenzene was added. The solution was stirred at room temperature for one hour, and refluxed for 2 hours. Then, 10% hydrochloric acid was added to the reactant solution, it was extracted with ethyl acetate. The organic layer was washed with brine, dried with magnesium sulfate, and the solvent was evaporated, so that coarse crystals were obtained. The coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 7.72 g of the titled compound was obtained (at a yield of 66%).

Quelle