反应详情

A mixture of 4-methylidene-3-(pent-4-en-1-yl)tetrahydro-2H-pyran (0.198 g, 1.19 mmol) in CH2Cl2 (20 mL) was degassed (3×N2/pump). Zhan-Ib (0.044 g, 0.060 mmol) was added, the reaction was degassed again, and stirred at rt for 1 hr. The resulting mixture was concentrated and purified by silica gel chromatography to provide the title compound. 1H NMR (500 MHz, CDCl3) δ 5.47 (s, 1H), 3.90-4.10 (m, 2H), 3.26-3.35 (m, 1H), 2.94 (t, 1H, J=11.0 Hz), 2.24-2.40 (m, 2H), 1.74-2.07 (m, 3H), 1.65-1.76 (m, 2H), 1.38-1.49 (m, 1H), 0.96-1.07 (m, 1H).

1. customwas degassed (3×N2/pump)
2. additionZhan-Ib (0.044 g, 0.060 mmol) was added
3. customthe reaction was degassed again
4. concentrationThe resulting mixture was concentrated
5. custompurified by silica gel chromatography