反应详情

温度

45 °C

To a solution of 1-difluoromethoxy-4-((E,Z)-2-methoxyvinyl)-benzene (E/Z ratio ˜3:2,) (1.58 g, 7.9 mmol, from step (i) above ) in acetone (20 mL) was added 3 M HCl (3.7 mL, 11.1 mmol) and the solution was stirred at 45° C. for 4 h. After concentration under reduced pressure, water (25 mL) was added to the residue and the aqueous phase was extracted with diethylether (2×50 mL). The combined organic phase was washed with saturated aqueous NaHCO3 (50 mL) and brine (50 mL), dried over Na2SO4, and concentrated in vacuo to give 1.32 g of crude product as a yellow oil with a purity of ca. 80%. The crude product was used directly in the subsequent reduction step without further purification.

1. concentrationAfter concentration under reduced pressure, water (25 mL)
2. additionwas added to the residue
3. extractionthe aqueous phase was extracted with diethylether (2×50 mL)
4. washThe combined organic phase was washed with saturated aqueous NaHCO3 (50 mL) and brine (50 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo