反应详情

To a stirred solution of 4-(4-iodo-phenyl)-4-(isobutoxycarbonylamino-methyl)-piperidine-1-carboxylic acid tert-butyl ester (0.075 g, 0.15 mmol) in CH2Cl2 (1.5 mL) at 0° C. was added TFA (0.5 mL). 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 [4-(4-iodo-phenyl)-piperidin-4-ylmethyl]-carbamic acid isobutyl ester as a reddish solid (0.058 g, ˜0.14 mmol). MS (ESI): 417.1/418.1(M+1).

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