反应详情

The solution of compound 12 (30.5 g, 0.1 mol) in CH2Cl2 (300 mL) at −78° C. was bubbled with O3 until the solution turned gray-blue. Then PPh3 (40 g, 0.15 mol) was added slowly to quench the reaction. After concentration, the residue was purified by column chromatography on silica gel (PE: EA=10:1) to give compound 13 (11 g, 35.8%). 1H NMR (400 MHz, CDCl3) δ 1.37 (s, 9 H), 3.57-3.61 (d, 1 H, J=18 Hz), 3.71 (s, 3H), 3.98-4.12 (m, 1 H), 6.16 (bs, 1 H), 7.31-7.43 (m, 5 H), 9.74 (s, 1H).

1. customto quench
2. customthe reaction
3. concentrationAfter concentration
4. customthe residue was purified by column chromatography on silica gel (PE: EA=10:1)