تفاعل #1997

معادلة التفاعل

hydrochloric acid

N,N-dimethylformamide

benzonitrile

sodium azide

→

product

المردود 90.1%

5-Phenyltetrazole

المردود 90.1%

المذيبات

water

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر