反应详情

温度

60 °C

A mixture comprised of Ni[P(O-tolyl)3]4 (3.3 g, 2.2 mmole) and P(O-tolyl)3 (1.7 g, 4.8 mmole), 2,2-bis(trifluoromethyl)-4-vinyl-4,5,5-trifluoro-1,3-dioxolane (30 g, 0.103 mole), 25% EtAlCl2 in toluene (2.0 ml), and toluene (25 ml) was heated under nitrogen in an oil bath at 60° C. A 50% HCN in toluene solution was fed from an ISCO pump at a rate of 1.5 ml/hour for 4.5 hours and then 0.5 ml/hour overnight until the reaction was complete (GC determination). The mixture was allowed to cool and was purified by distillation to give 2,2- bis(trifluoromethyl)-4-(2-cyanoethyl)-4,5,5-trifluoro1,3-dioxolane as a clear, colorless liquid in 66% yield. Bp. 65°-68° C./7.0 mm. 1H-NMR (CDCl3): δ 2.72 (t, J=7.8 Hz, 2H), 2.50 (m, 2H); 19F NMR (CDCl3 ): -110.2 (m, 1F), -76.9, -77.6 (2m, 1F), -87.0, -87.7 (2d, J=9.3 Hz, 1F), -80.6 (m, 3F), -81.3 (m, 3F). Anal. Calc. for C8H4F9NO2 : C: 30.28, H: 1.27, F: 53.94; Found: 30.21, H: 1.34, F: 54.26. MS: [M]: Calc.: 317.0098; Found: 317.0081; MS (PCI): [M+H]: Calc.: 318.0177; Found: 318.0176. ##STR10##

1. custom0.5 ml/hour overnight
2. temperatureto cool
3. distillationwas purified by distillation