反应详情

172 mg of 3-amino-4-(2,2-dimethoxyethyl)benzamide and 127 mg of 1-(2-(1-acetyl-6-methoxy-1,2,3,4-tetrahydroquinolin-7-yl)ethyl)piperidin-4-one were dissolved in 5 ml of acetic acid. Thereafter, 0.65 g of sodium sulfate was added to the reaction solution, and the obtained mixture was then stirred at room temperature for 1 hour. Thereafter, 0.16 g of sodium triacetoxyborohydride was added to the reaction solution, and the obtained mixture was then stirred for 1 hour. Thereafter, 5 ml of water was added thereto, and the obtained mixture was then stirred at 100° C. for 2 hours. The reaction solution was cooled to a room temperature, and it was then concentrated under a reduced pressure. A saturated sodium bicarbonate aqueous solution was added to the residue, followed by extraction with chloroform. The extract was dried over magnesium sulfate and then concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (chloroform-methanol) and NH silica gel column chromatography (ethyl acetate-methanol), so as to obtain 146 mg of the subject compound.

1. stirringthe obtained mixture was then stirred for 1 hour
2. stirringthe obtained mixture was then stirred at 100° C. for 2 hours
3. temperatureThe reaction solution was cooled to a room temperature
4. concentrationit was then concentrated under a reduced pressure
5. additionA saturated sodium bicarbonate aqueous solution was added to the residue
6. extractionfollowed by extraction with chloroform
7. dry with materialThe extract was dried over magnesium sulfate
8. concentrationconcentrated under a reduced pressure
9. customThe residue was purified by silica gel column chromatography (chloroform-methanol) and NH silica gel column chromatography (ethyl acetate-methanol)