反应详情

温度

120 °C

To a solution of 4-(3-cyanophenoxazin-10-yl)-piperidine-1-carboxylic acid tert-butyl ester, 4a (0.29 g; 0.68 mmol) in DMF (7 mL) were added sodium azide (0.13 g, 2.0 mmol) and ammonium chloride (0.11 g; 2.06 mmol), and the mixture was heated at 120° C. for 16 h. The mixture was allowed to cool to rt, and filtered. The filtrate was acidified with 1N hydrochloric acid (10 mL) and extracted with ethyl acetate (3×10 mL). The combined organic layers were dried over MgSO4, filtered, and evaporated, yielding 4-[3-(1H-tetrazol-5-yl)-phenoxazin-10-yl]-piperidine-1-carboxylic acid tert-butyl ester, 5a. MS m/z (M+Na) 456.9. The crude material was used as such for the next reaction.

1. temperatureto cool to rt
2. filtrationfiltered
3. extractionextracted with ethyl acetate (3×10 mL)
4. dry with materialThe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. customevaporated