反应详情

To a solution of 0.95 g (0.0045 mole) of 4-fluoro-4,4-dinitrobutyryl chloride in 20 mL of anhydrous diethyl ether stirred at 20° C. was added 0.8 g (0.0045 mole) of N-(perfluoropropionyl)hydrazine followed by the dropwise addition of 0.4 mL of pyridine. After 5 minutes, dilute hydrochloric acid (10 mL) was added, the ether layer was separated, dried (Na2SO4) and the volatiles were removed to give the product N-(4-fluoro-4,4-dinitrobutyryl)-N'-(perfluoropropionyl)hydrazine, 1.05 g, mp 128°-132° C. Crystallization from 1,2-dichloroethane gave 0.93 g (58%), mp 135°-136° C. 1H NMR (acetone d6 +D2O): 2.80 (t, 2H), 3.36, 3.58 (d of t, 2H).

1. customthe ether layer was separated
2. dry with materialdried (Na2SO4)
3. customthe volatiles were removed