反应详情

温度

135 °C

A mixture of 2,2,3,3,4,4,5,5,5-nonafluoro-N-[4-(cyanomethyl)phenyl]pentanamide (6.8 g), sodium azide (5.56 g), ammonium chloride (4.53 g) and dimethylformamide (100 mL) were heated in a 135° C. oil bath under a nitrogen atmosphere overnight. Enough water was added to the hot reaction mixture to dissolve all suspended salts, the mixture was cooled to room temperature and more water was added until a precipitate formed. The solid was collected, washed with water and air dried. Recrystallization from ethylacetate/diethyl ether mixture yielded 3.4 g of the title compound as white flakes, m.p. 173°-174° C. The filtrate produced a second crop of 1.1 g of the title compound.

1. dissolutionto dissolve all suspended salts
2. temperaturethe mixture was cooled to room temperature
3. customformed
4. customThe solid was collected
5. washwashed with water and air
6. customdried
7. customRecrystallization from ethylacetate/diethyl ether mixture