反应详情

Heat a mixture of 25 gm. (0.106 mole) of 2-cyano-6,11-dihydro-11-oxodibenz[b,e]oxepin, 8.28 gm. (0.127 mole of sodium azide and 7.37 gm. (0.138 mole of ammonium chloride in 250 ml. of N,N-dimethylformamide to 140° C. for 27 hours. Cool, dilute with 500 cc. of water and acidify with 20% aqueous hydrochloric acid. Separate the solids by filtration and crystallize from ethanol to obtain the title product (m.p. 248° C. dec.).

1. temperatureHeat
2. additiona mixture of 25 gm
3. temperatureCool
4. additiondilute with 500 cc
5. customSeparate the solids
6. filtrationby filtration
7. customcrystallize from ethanol