Hydrazine → HCID 10252560, compound

Participants

Reaction Steps

A mixture of 1,10-diazido-3-trifluoromethyl-3,4,4,5,5,6,6,7,7,8,8-undecafluorodecane (7.2 g, 14.7 mmol), methanol (40 mL), Pearlman's catalyst (0.6 g) and a solution of hydrazine (1.1 g, 36 mmol) in methanol (5 mL) was heated under reflux for 21 hours. The mixture was diluted with methanol and filtered through a pad of celite. Methanol was evaporated and the residue was distilled to give 2.5 g (39%) of 1,10-diamino-3-trifluoromethyl-3,4,4,5,5,6,6,7,7,8,8-undecafluorodecane, a colorless oil; bp 0.2 mm, 85°-95° C./0.2 mm; Glc (OV-17, 110° C. to 260° C. at 16° C./min) RT 5.4 min; IR (neat) 3350, 3050, 2975 and 1050-1380 cm-1 ; 1H NMR (CDCl3) δ 3.0 (t, J=6 Hz, 4H), 2.20 (m, 4H) and 1.23 (s, 4H). Anal Calcd for C11H12F 14 N2 : C, 30.15; H, 2.76; F, 60-70. Found: C, 29.85; H, 2.36; F, 60.32.

Provenance & Evidence