反应 #1997

反应方程式

hydrochloric acid

N,N-dimethylformamide

benzonitrile

sodium azide

→

product

收率 90.1%

5-Phenyltetrazole

收率 90.1%

溶剂

water

反应条件

后处理

1. 1
   温度while maintaining the temperature below 60° C
2. 2
   温度The heterogeneous mixture was heated at 115° C. with agitation for 18 hours
3. 3
   温度The mixture was cooled to room temperature
4. 4
   温度The mixture was cooled to 0° C. and aged for one hour
5. 5
   过滤filtered
6. 6
   洗涤the filter cake washed with 15 mL of cold 0.1N HCl
7. 7
   其他then dried at 60° C. under vacuum

实验过程

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.

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