反应详情

A mixture formed by adding 0.77 g (0.0043 mole) of N-(perfluoropropionyl)hydrazine to a solution of 1.05 g (0.0043 mole) of 4,4,4-trinitrobutyryl chloride in 30 mL of anhydrous diethyl ether was stirred at 20° C during the dropwise addition of 0.35 mL of pyridine. After 5 minutes, dilute hydrochloric acid (10 mL) was added, and the ether layer was separated and dried (MgSO4). Removal of volatiles gave a semisolid which was stirred with dilute sodium bicarbonate to give 1.0 g, mp 105°-118° C. Crystallization from 1,2-dichloroethane gave the product, N-(4,4,4-trinitrobutyryl)-N'-(perfluoropropionyl)hydrazine, 0.65 g (41%), mp 123°-125° C.; 1H NMR (acetone-d6 +D2O): 2.95 (t, 2H); 3.85 (t, 2H).

1. customA mixture formed
2. customthe ether layer was separated
3. dry with materialdried (MgSO4)
4. customRemoval of volatiles
5. customgave a semisolid which
6. customto give 1.0 g, mp 105°-118° C
7. customCrystallization from 1,2-dichloroethane