反应详情

Potassium carbonate (0.033 mg) and isopropyl iodide (0.024 mL) were sequentially added to an acetonitrile (1.9 mL) suspension of methyl 2-(2-(benzyloxy)-5-(piperidin-4-yl)benzamido)-4-phenylbenzoate (0.13 g), followed by heating to reflux for 1 hour. The reaction mixture was cooled to room temperature, and potassium carbonate (6.7 mg) and isopropyl iodide (4.8 μL) were sequentially added thereto, followed by heating to reflux for 2 hours. After cooling the reaction mixture to room temperature, the solvent was evaporated under reduced pressure, and ethyl acetate and a saturated aqueous solution of sodium bicarbonate were added to the residue. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 100-95% chloroform/methanol] to obtain 0.12 g of methyl 2-(2-(benzyloxy)-5-(1-isopropylpiperidin-4-yl)benzamido)-4-phenylbenzoate as an orange oily sub stance.

1. temperatureby heating
2. temperatureto reflux for 1 hour
3. temperatureby heating
4. temperatureto reflux for 2 hours
5. temperatureAfter cooling the reaction mixture to room temperature
6. customthe solvent was evaporated under reduced pressure, and ethyl acetate
7. additiona saturated aqueous solution of sodium bicarbonate were added to the residue
8. customThe organic layer was separated
9. washwashed with a saturated aqueous solution of sodium chloride
10. dry with materialdried over anhydrous sodium sulfate
11. customthe solvent was evaporated under reduced pressure
12. customThe obtained residue was purified by silica gel column chromatography [eluent: 100-95% chloroform/methanol]