反应详情

41.6 g of AlCl3 were suspended in 400 mL of dichloromethane. At room temperature, a solution of 22.95 g of N-(2,2-Dimethoxy-ethyl)-N-(4-fluoro-benzyl)-4-methyl-benzenesulfonamide (22) in 150 ml of dichloromethane was added. Stirring was continued at room temperature overnight, the solution was poured on ice, the organic layer was separated, the aqueous phase was extracted twice with dichloromethane and the combined organic layers are then extracted twice with sodium bicarbonate. The organic layer was dried over magnesium sulfate, evaporated to dryness and the obtained crude product (8.75 g) is purified by silica gel chromatography to yield 2.74 g of compound 23. Rt=0.30 min (Method #4). Detected mass: 148.1 (M+H+).

1. additionthe solution was poured on ice
2. customthe organic layer was separated
3. extractionthe aqueous phase was extracted twice with dichloromethane
4. extractionthe combined organic layers are then extracted twice with sodium bicarbonate
5. dry with materialThe organic layer was dried over magnesium sulfate
6. customevaporated to dryness
7. customthe obtained crude product (8.75 g)
8. customis purified by silica gel chromatography