反应详情

A mixture of 5-(4-cyanobutyl)-imidazo[1,5-a]pyridine (4.0 g), sodium azide (1.88 g), ammonium chloride (1.57 g) and lithium chloride (10 mole %) in 14 ml of dry dimethylformamide is heated at 125° for 17 hours. The reaction mixture is cooled, filtered and evaporated to a residual oil which is redissolved in 50 ml of water and extracted with ethyl acetate (50 ml). The aqueous phase is adjusted to pH=2 and extracted with ethyl acetate and then adjusted to pH=5. The resulting solid is collected by filtration and converted to its hydrochloride salt which is recrystallized from acetone/methanol to yield 5-[4-(5-tetrazolyl)butyl]-imidazo[1,5-a]pyridine monohydrochloride, m.p. 159°-161°.

1. temperatureis heated at 125° for 17 hours
2. temperatureThe reaction mixture is cooled
3. filtrationfiltered
4. customevaporated to a residual oil which
5. dissolutionis redissolved in 50 ml of water
6. extractionextracted with ethyl acetate (50 ml)
7. extractionextracted with ethyl acetate
8. filtrationThe resulting solid is collected by filtration
9. customis recrystallized from acetone/methanol