反应详情

A mixture of (2-methylidenecyclohexyl)methyl prop-2-en-1-yl ether (0.104 g, 0.626 mmol) in DCE (6.5 mL) was degassed 3×N2/pump, then Zhan-1b (0.023 g, 0.031 mmol) was added and the reaction was degassed again The mixture was stirred at rt for 2 hr. It was concentrated and purified by silica gel chromatography to provide the title compound. 1H NMR (500 MHz, CDCl3) δ 5.39 (t, 1H, J=2.4 Hz), 4.04-4.10 (m, 2H), 3.92 (dd, 1H, J=5.7 Hz, 11.2 Hz), 3.24 (dd, 1H, J=8.2 Hz, 11.2 Hz), 2.15-2.27 (m, 2H), 1.92-2.02 (m, 1H), 1.74-1.83 (m, 2H), 1.64-1.72 (m, 1H), 1.18-1.45 (m, 2H), 0.93-1.06 (m, 1H).

1. customwas degassed 3×N2/pump
2. additionZhan-1b (0.023 g, 0.031 mmol) was added
3. customthe reaction was degassed again The mixture
4. concentrationIt was concentrated
5. custompurified by silica gel chromatography