反应详情

H2SO4 (1.45 mL) was added dropwise to 4-(2,2′-bithiophene-3-yl)-2,6-dimethylheptan-4-ol (IIb) (0.688 g, 2.23 mmol) under stirring at room temperature. After stirring for 12 h, CH2Cl2 (15 mL) and water (15 mL) were added. The organic layer was separated and the aqueous layer was extracted with CH2Cl2. The combined organic extracts were successively washed with saturated NaHCO3 and brine. After drying over MgSO4, the solvent was removed in vacuo. The crude oil was purified with column chromatography (eluent hexane) to afford a pure dark yellow oil (Ib) (0.240 g, 35.0%). 1H-NMR (CDCl3): δ=7.12 (d, J=4.8 Hz, 2H), 6.92 (d, J=4.8 Hz, 2H), 1.85 (d, J=5.8 Hz, 4H), 1.08-0.78 (m, 2H), 0.50 (d, J=7.1 Hz, 12H). 13C-NMR (CDCl3): δ=158.45, 137.29, 124.99, 122.66, 53.69, 49.30, 25.46, 25.14.

1. stirringAfter stirring for 12 h
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with CH2Cl2
4. washThe combined organic extracts were successively washed with saturated NaHCO3 and brine
5. dry with materialAfter drying over MgSO4
6. customthe solvent was removed in vacuo
7. customThe crude oil was purified with column chromatography (eluent hexane)
8. customto afford a pure dark yellow oil (Ib) (0.240 g, 35.0%)