反应详情

A mixture of 1-(but-3-en-1-yloxy)-2-methylidenecyclohexane (5.21 g, 31.3 mmol) in DCE (313 mL) was degassed 3×N2/pump. Zhan-1b (1.15 g, 1.57 mmol) was then added and the reaction was degassed again. The reaction was stirred at rt for 2 hr. The reaction mixture was concentrated and the residue was purified by column chromatography to give the title compound. 1H NMR (500 MHz, CDCl3) δ 5.48 (d, 1H, J=2.7 Hz), 3.90-3.96 (m, 2H), 3.50-3.60 (m, 1H), 2.18-2.34 (m, 2H), 2.02-2.08 (m, 1H), 1.84-1.99 (m, 2H), 1.76-1.83 (m, 1H), 1.66-1.74 (m, 1H), 1.15-1.43 (m, 3H).

1. customwas degassed 3×N2/pump
2. additionZhan-1b (1.15 g, 1.57 mmol) was then added
3. customthe reaction was degassed again
4. concentrationThe reaction mixture was concentrated
5. customthe residue was purified by column chromatography