反应详情

To a solution of 4-chlorobenzenethiol (5.78 g; 40 mmol) in anhydrous acetone (50 mL) was added potassium carbonate (5.52 g, 40 mmol) and dropwise at room temperature 2-bromo-1,1-dimethoxy-ethane (4.7 mL, 40 mmol). After 24 h of stirring, the precipitate was filtered, the filtrate concentrated, the residue diluted with water and diethyl ether (150 mL), the organic layer washed successively with water (60 mL), NaOH 4N (30 mL) and water (60 mL), dried over Na2SO4 and concentrated to give 1-chloro-4-(2,2-dimethoxy-ethylsulfanyl)-benzene (compound PRE9) (9.12 g; orange oil) (Yield=98%).

1. customdropwise at room temperature
2. filtrationthe precipitate was filtered
3. concentrationthe filtrate concentrated
4. additionthe residue diluted with water and diethyl ether (150 mL)
5. washthe organic layer washed successively with water (60 mL), NaOH 4N (30 mL) and water (60 mL)
6. dry with materialdried over Na2SO4
7. concentrationconcentrated