反应详情

To a solution of crude 2,4-dichloro-N-[2-chloro-4-(tetrahydro-pyran-2-yloxy)-benzyl]-N-[4-(2-pyrrolidin-1-yl-ethoxy)-phenyl]-benzenesulfonamide (0.096 g, 0.15 mmol) in 4 mL absolute ethanol was added 1 mL of 1.2N HCl. The reaction mixture was stirred at room temperature for 24 hr. and was diluted with 10 mL saturated aqueous sodium bicarbonate. The aqueous solution was washed with methylene chloride (2×10 mL). The combined organic layers were dried (sodium sulfate), filtered, and concentrated. The residue was purified by preparative TLC (1.0 mm silica gel layer, elution with 10% methanol/ethyl acetate) to afford 0.029 g of the title compound. MS 557.3 (M+1)+

1. washThe aqueous solution was washed with methylene chloride (2×10 mL)
2. dry with materialThe combined organic layers were dried (sodium sulfate)
3. filtrationfiltered
4. concentrationconcentrated
5. customThe residue was purified by preparative TLC (1.0 mm silica gel layer, elution with 10% methanol/ethyl acetate)