反应详情

温度

0 °C

Step 3): A mixture of 5-isopropyl-N-tert-butoxycarbonylanthranilic acid (1.0 g, 3.58 mmol), 4-aminomethyl-1-diphenylmethylpiperidine (1.0 g, 3.57 mmol), triethylamine (0.37 g, 3.66 mmol) and DPPA (1.0 g, 3.63 mmol) in DMF was stirred at 0° C. for 30 mins and at room temperature for 2 hours. The mixture was poured into H2O and extracted with AcOEt. The extract was washed with H2O, dried over MgSO4 and evaporated and then the residue was purified by column chromatography on silica gel to give 2-(tert-butoxycarbonyl)amino-5-isopropyl-N-[(1-diphenylmethylpiperidin-4-yl)methyl]benzamide, 1.86 g (96.4%): mp 88°-90° C.

1. extractionextracted with AcOEt
2. washThe extract was washed with H2O
3. dry with materialdried over MgSO4
4. customevaporated
5. customthe residue was purified by column chromatography on silica gel