反应详情

To a solution of 2B (3.637 g, 13.3 mmol) in methanol was added dropwise at 0° C. a solution of NaBH4 added to 3.9 g NaOH dissolved in 7.8 mL H2O. The solution was allowed to stir at room temperature overnight. Water was added and the product was extracted with ether (2×) and washed with brine (2×). The combined ether extracts were dried over MgSO4. The solvent was removed and the product was purified using flash chromatography with a hexanes and then ethyl acetate. The ethyl acetate fraction was collected and the solvent removed to reveal 2.667 g (74%) of a honey yellow crystal solid. 1H NMR (CDCl3): δ4.63 (d, 2H), δ6.97–7.06 (m, 6H), δ7.09 (m, 2H), δ7.20–7.28 (m, 6H); m/z 298.1 (M++Na), 276.1 (M++H), 258.1 (M+−H2O).

1. extractionthe product was extracted with ether (2×)
2. washwashed with brine (2×)
3. dry with materialThe combined ether extracts were dried over MgSO4
4. customThe solvent was removed
5. customthe product was purified
6. customThe ethyl acetate fraction was collected
7. customthe solvent removed