反应详情

温度

80 °C

A vigorously stirred mixture of 1-(4-hydroxy-2,6-dimethylphenyl)ethanone (4-2, 1.00 g, 10.9 mmol), chloromethylcyclopropane (4-1, 1.22 g, 7.4 mmol), and powdered potassium carbonate (1.54 g, 11.1 mmol) in DMF (10.0 mL) was heated at 80° C. for 16 h under N2. The mixture was allowed to cool and was filtered through Diatomaceous earth. The filtrate was concentrated under reduced pressure and the residue was extracted with EtOAc. The organic layer was washed with saturated aqueous sodium carbonate and dried over Na2SO4. The solution was concentrated under reduced pressure to provide 1-(4-(cyclopropylmethoxy)-2,6-dimethylphenyl)ethanone (4-3, 1.61 g) as off-white solids in 99% yield: 1H NMR (500 MHz, CDCl3) δ 6.55 (s, 2 H), 3.77 (d, J=6.9 Hz, 2 H), 2.45 (s, 3 H), 2.27 (s, 6 H), 1.19 (s, 1 H), 0.64 (m, 2 H), 0.33 (m, 2 H).

1. temperatureto cool
2. filtrationwas filtered through Diatomaceous earth
3. concentrationThe filtrate was concentrated under reduced pressure
4. extractionthe residue was extracted with EtOAc
5. washThe organic layer was washed with saturated aqueous sodium carbonate
6. dry with materialdried over Na2SO4
7. concentrationThe solution was concentrated under reduced pressure