反应详情

1-(2,2-Diethoxyethylsulphanyl)-3-methoxybenzene (18 g, 70.21 mmol), glacial acetic acid (26 mL) and water (18 mL) were stirred at reflux temperature under nitrogen for 45 min. The reaction mixture was cooled to ambient temperature, diluted with water (180 mL) and extracted with tert-butyl methyl ether (3×40 mL). The combined extracts were cooled to <5° C. and washed with 5% aqueous sodium carbonate solution, water, and brine. The organic phase was dried (MgSO4) and concentrated in vacuo to yield the title compound (11.8 g, 92%).

1. temperatureat reflux temperature under nitrogen for 45 min
2. extractionextracted with tert-butyl methyl ether (3×40 mL)
3. temperatureThe combined extracts were cooled to <5° C.
4. washwashed with 5% aqueous sodium carbonate solution, water, and brine
5. dry with materialThe organic phase was dried (MgSO4)
6. concentrationconcentrated in vacuo