反应详情

To a solution of 4-[3-(3,5-dichloro-phenyl)-1-methyl-ureidomethyl]-4-(4-iodo-phenyl)-piperidine-1-carboxylic acid tert-butyl ester (0.218 g, 0.35 mmol) in CH2Cl2 (4.5 mL) at 0° C. was added TFA (1.5 mL, to give a 25% v/v solution). The reaction mixture was warmed to room temperature and stirred for 4 h. The solvent was removed by rotary evaporation and the residue was dissolved in EtOAc (25 mL) and washed with 10% aqueous NaHCO3 (2×25 mL). The organic extracts were dried over anhydrous Na2SO4, filtered and concentrated by rotary evaporation to give 3-(3,5-dichloro-phenyl)-1-[4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-1-methyl-urea (˜0.19 g, 100%).

1. customto give a 25% v/v solution)
2. customThe solvent was removed by rotary evaporation
3. dissolutionthe residue was dissolved in EtOAc (25 mL)
4. washwashed with 10% aqueous NaHCO3 (2×25 mL)
5. dry with materialThe organic extracts were dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated by rotary evaporation