反应详情

温度

130 °C

A mixture of 2,2,3,3,4,4,4-heptafluoro-N-[2-(cyanomethyl)phenyl]butanamide (15 g), sodium azide (14.85 g), ammonium chloride (12.22 g) and dimethylformamide (200 mL) was heated in a 130° C. oil bath under a nitrogen atmosphere overnight. The reaction mixture was cooled to room temperature, water (100 mL) was added and the product was extracted with ethylacetate (3×200 mL). The combined extracts were dried over Na2SO4, filtered and concentrated with a rotary evaporator. The brown residue was purified by high pressure liquid chromatography to give a white solid. The solid was triturated with diethyl ether to give 3.2 g of the title compound, m.p. 117°-178° C.

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionthe product was extracted with ethylacetate (3×200 mL)
3. dry with materialThe combined extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated with a rotary evaporator
6. customThe brown residue was purified by high pressure liquid chromatography
7. customto give a white solid
8. customThe solid was triturated with diethyl ether