反应详情

To 50 mg (0.14 mmol) of 1-9 in 1 mL of CH2Cl2 was added 71 mg (0.17 mmol) of Dess-Martin Periodinane (Lancaster Synthesis) and the mixture was left to stir for 15 min at room temperature. The reaction was diluted with 10 mL of CH2Cl2, quenched with 5 mL of 5% aqueous NaHSO3 and 10 mL of saturated aqueous NaHCO3 and the biphasic mixture was stirred for 30 min. The layers were separated, the organic was washed with NaHCO3 and water, dried over Na2SO4, and concentrated to provide 3-1 as a white solid. Data for 3-1: 1HNMR (500 MHz, CDCl3) δ 9.6 (s, 1H), 7.4-7.2 (m, 5H), 7.1-6.9 (m, 3H), 6.2 (s, 1H), 4.9 (d, 1H), 4.8 (d, 1H), 3.0 (s, 6H) ppm.

1. waitthe mixture was left
2. customquenched with 5 mL of 5% aqueous NaHSO3 and 10 mL of saturated aqueous NaHCO3
3. stirringthe biphasic mixture was stirred for 30 min
4. customThe layers were separated
5. washthe organic was washed with NaHCO3 and water
6. dry with materialdried over Na2SO4
7. concentrationconcentrated