反应详情

温度

22 °C

4-(3-tert-Butoxycarbonylamino-phenoxy)-piperidine-1-carboxylic acid benzyl ester (11.8 g, 27.6 mmol) is dissolved in a solution of trifluoroacetic acid in dichloromethane (25% v/v, 20 mL). The reaction mixture is stirred at 22° C. for 60 min. After removal of the solvent, the oily residue is dissolved in dichloromethane (250 mL) and neutralized with 0.2 N aqueous sodium hydroxide solution (250 mL) and extracted with dichloromethane (10×100 mL) followed by ethyl acetate (5×100 mL). The combined organic phases are dried over anhydrous sodium sulfate. After removal of solvent, the crude product is purified on silica gel chromatography with dichloromethane-methanol to give a light brown oil (4.84 g, 54%, ES+(m/z) 327.3 [M+H]).

1. customAfter removal of the solvent
2. dissolutionthe oily residue is dissolved in dichloromethane (250 mL)
3. extractionextracted with dichloromethane (10×100 mL)
4. dry with materialThe combined organic phases are dried over anhydrous sodium sulfate
5. customAfter removal of solvent
6. customthe crude product is purified on silica gel chromatography with dichloromethane-methanol
7. customto give a light brown oil (4.84 g, 54%, ES+(m/z) 327.3 [M+H])