反应详情

To a stirred solution of 4-[(3-chloro-4-fluoro-benzenesulfonylamino)-methyl]-4-(4-iodo-phenyl)-piperidine-1 carboxylic acid tert-butyl ester (0.09 g, 0.16 mmol) in CH2Cl2 (1.5 mL) at 0° C. was added TFA (0.5 mL, to give a 25% v/v solution). The mixture was stirred at room temperature for 3 h. TLC (4:1 hexanes/EtOAc) showed no starting material left. The solvent was removed by rotary evaporation and the resulting liquid was evaporated from toluene (2×10 mL), diluted with EtOAc (100 mL) and washed with 10% aqueous NaHCO3 solution (2×50 mL) and saturated brine (50 mL). The organic layer was dried over anhydrous Na2SO4, filtered, concentrated by rotary evaporation, and dried under high vacuum for 1 h to give 3-chloro-4-fluoro-N-[4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-benzenesulfonamide as a reddish solid (0.021 g, ˜0.04 mmol). MS: 509/511 (M+1).

1. customto give a 25% v/v solution)
2. waitleft
3. customThe solvent was removed by rotary evaporation
4. customthe resulting liquid was evaporated from toluene (2×10 mL)
5. additiondiluted with EtOAc (100 mL)
6. washwashed with 10% aqueous NaHCO3 solution (2×50 mL) and saturated brine (50 mL)
7. dry with materialThe organic layer was dried over anhydrous Na2SO4
8. filtrationfiltered
9. concentrationconcentrated by rotary evaporation
10. customdried under high vacuum for 1 h