反应详情

Under vigorous stirring, at rt, 8-benzylidene-1,4-dioxaspiro-[4.5]-decane (1.8 g, 7.81 mmol) was dissolved in a acetone/HCl (10% v/v) mixture (70 mL:35 mL) and left to stir 4 h. The crude mixture was diluted in water and extracted with AcOEt (3×40 mL). The combined organic fractions were washed with brine, dried over Na2SO4, filtered and concentrated to dryness to afford pure title compound (1.4 g, 96%) as colorless oil. 1H NMR (CDCl3): δ 2.44 (t, J=7.0 Hz, 2H), 2.53 (t, J=6.8 Hz, 2H), 2.65-2.72 (m, 2H), 2.74-2.80 (m, 2H), 6.49 (s, 1H), 7.21-7.27 (m, 3H), 7.32-7.39 (m, 2H).

1. waitleft
2. extractionextracted with AcOEt (3×40 mL)
3. washThe combined organic fractions were washed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated to dryness