반응 #1997

반응 방정식

hydrochloric acid

N,N-dimethylformamide

benzonitrile

sodium azide

→

product

수율 90.1%

5-Phenyltetrazole

수율 90.1%

용매

water

반응 조건

후처리

1. 1
   온도while maintaining the temperature below 60° C
2. 2
   온도The heterogeneous mixture was heated at 115° C. with agitation for 18 hours
3. 3
   온도The mixture was cooled to room temperature
4. 4
   온도The mixture was cooled to 0° C. and aged for one hour
5. 5
   여과filtered
6. 6
   세척the filter cake washed with 15 mL of cold 0.1N HCl
7. 7
   기타then dried at 60° C. under vacuum

실험 절차

Zinc chloride (3.3 g, 24.3 mmol, 0.5 eq) was added to 15 mL of N,N-dimethylformamide in small portions while maintaining the temperature below 60° C. The suspension of zinc chloride was cooled to room temperature and treated with 5.0 g of benzonitrile (48.5 mmol, 1.0 eq) followed by 3.2 g of sodium azide (48.5 mmol, 1.0 eq). The heterogeneous mixture was heated at 115° C. with agitation for 18 hours. The mixture was cooled to room temperature, water (30 mL) was added and the mixture acidified by the addition of 5.1 mL of concentrated hydrochloric acid. The mixture was cooled to 0° C. and aged for one hour, then filtered and the filter cake washed with 15 mL of cold 0.1N HCl then dried at 60° C. under vacuum to afford 6.38 g (43.7 mmol, 90%) of the product.

출처