反应详情

To a mechanically stirred suspension of 95.2 g (699.5 mmol) AlCl3 in 400 ml dichloromethane a solution of 59.9 g (139.8 mmol) N-(4-Bromo-benzyl)-N-(2,2-dimethoxy-ethyl)-4-methyl-benzenesulfonamide (2) in 400 ml dichloromethane was added and the reaction was stirred at room temperature for 4 h. After standing overnight, the reaction mixture was poured on ice, the organic layer was separated and the aqueous layer was extracted twice with dichloromethane. The combined dichloromethane solutions were washed with 1 N NaOH (2×) and saturated NaHCO3-solution (2×). After drying with MgSO4 and evaporation of the solvent, the crude product was purified by silicagel chromatography (heptane/ethyl acetate 1:1) to yield 17.5 g of the title compound. Rt=0.68 min (Method C). Detected mass: 208.1/210.1 (M+H+).

1. additionwas added
2. waitAfter standing overnight
3. additionthe reaction mixture was poured on ice
4. customthe organic layer was separated
5. extractionthe aqueous layer was extracted twice with dichloromethane
6. washThe combined dichloromethane solutions were washed with 1 N NaOH (2×) and saturated NaHCO3-solution (2×)
7. dry with materialAfter drying with MgSO4 and evaporation of the solvent
8. customthe crude product was purified by silicagel chromatography (heptane/ethyl acetate 1:1)