反应详情

温度

80 °C

To a solution of 2 (3.4 g, 9.99 mmol) in MeOH (85 ml) was added 2N NaOH (50 ml), and the mixture was stirred at 80° C. for 15 h. After cooling, 2 N HCl (50 ml) was added drop wise under ice cooling, and the whole was extracted with AcOEt, the organic layer was washed with brine, dried over Na2SO4, then concentrated. The residual solid was triturated with hexanes to give 3 (88%). 3: colorless powder; 1H-NMR (CDCl3) δ 1.03 (3H, t, J=7.4 Hz), 2.81 (2H, q, J=7.4 Hz), 3.42 (3H, s), 5.08 (2H, s), 6.78 (2H, d, J=8.8 Hz), 6.94 (2H, d, J=8.8 Hz), 7.02 (2H, m), 7.11-7.19 (3H, m).

1. temperatureAfter cooling
2. extractionthe whole was extracted with AcOEt
3. washthe organic layer was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residual solid was triturated with hexanes