反应详情

A mixture of 2-thenoylacetonitrile (9 g, 59.3 mmol), Sodium azide (4.33 g, 66.7 mmol) and triethylammoniumchloride (9.14 g, 66.9 mmol) was stirred in dry toluene (139 mL) under argon atmosphere at 90° C. for 18 hrs. A two-phase system was formed, cooled and extracted with NaOH (2M, 3×500 mL), and the aqueous solution was poured into hydrochloric acid (4M, 300 mL) and the crude tetrazole was filtered off and recrystalised from acetonitrile. Yield: 43.5%.

1. customA two-phase system was formed
2. temperaturecooled
3. extractionextracted with NaOH (2M, 3×500 mL)
4. additionthe aqueous solution was poured into hydrochloric acid (4M, 300 mL)
5. filtrationthe crude tetrazole was filtered off
6. customrecrystalised from acetonitrile