反应详情

To a solution of crude tert-butyl 2-(4-(3-fluoro-2-methylbenzylcarbamoyl)-4-(hydroxymethyl)piperidin-1-yl)-2-oxoethylcarbamate (185 mg, ˜0.422 mmol, 1.0 equiv.) in THF (2 mL) were added DMAP (10 mg, 0.085 mmol, 0.2 equiv.) and 4-ethylphenylisocyanate (61 μL, 0.422 mmol, 1.0 equiv.). The reaction mixture was stirred overnight, and then concentrated. The resulting residue was purified on RP-HPLC using a mixture of acetonitrile and H2O to give (1-(2-(tert-butoxycarbonylamino)acetyl)-4-(3-fluoro-2-methylbenzylcarbamoyl)piperidin-4-yl)methyl 4-ethylphenylcarbamate (12 mg, 5% for three steps). LRMS (M-Boc+H+) m/z 485.2.

1. concentrationconcentrated
2. customThe resulting residue was purified on RP-HPLC
3. additiona mixture of acetonitrile and H2O