反应详情

温度

5 °C

Bis-(2-cyanoethyl)ether 186 g (1.5 mole), 215 g of sodium azide and 177 g of ammonium chloride were slurried in 1070 ml of dimethylformamide. The mixture was heated at 118°-122° C. with stirring and under reflux for 24 hr. (since ammonia and some ammonium azide are evolved, the heating should be done in a hood). After the bulk of the solvent had been removed at 80°-90° C. and 25 mm pressure, the residue was first heated to boiling with 500 ml of water and 40 ml of concentrated hydrochloric acid, then cooled to 5° C. (Caution: some hydrazoic acid is liberated). The product was filtered, washed twice with cold water and dried; 287 g (91%). Recrystallization of 5 g from 85 ml of water furnished coarse blades, m.p. 199°-200° C. (dec.).

1. temperatureThe mixture was heated at 118°-122° C.
2. temperatureunder reflux for 24 hr
3. customAfter the bulk of the solvent had been removed at 80°-90° C.
4. temperature25 mm pressure, the residue was first heated
5. filtrationThe product was filtered
6. washwashed twice with cold water
7. customdried
8. customRecrystallization of 5 g from 85 ml of water
9. customfurnished coarse blades, m.p. 199°-200° C. (dec.)