反应详情

129 mg of 3-amino-4-(2,2-dimethoxyethyl)benzamide and 87 mg of 1-(2-(6-methoxy-1-methyl-1,2,3,4-tetrahydroquinolin-7-yl)ethyl)piperidin-4-one were dissolved in 4 ml of acetic acid. Thereafter, 0.49 g of sodium sulfate was added to the reaction solution, and the obtained mixture was then stirred at room temperature for 1 hour. Thereafter, 0.12 g of sodium triacetoxyborohydride was added to the reaction solution, and the obtained mixture was then stirred at room temperature for 1 hour. Thereafter, 4 ml of water was further added to the reaction solution, and the obtained mixture was then stirred at 100° C. for 2 hours. The reaction solution was cooled to a room temperature, followed by concentration 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 (ethyl acetate-methanol) and by NH silica gel column chromatography (ethyl acetate), so as to obtain 70 mg of the subject compound.

1. stirringthe obtained mixture was then stirred at room temperature 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. concentrationfollowed by concentration 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 (ethyl acetate-methanol) and by NH silica gel column chromatography (ethyl acetate)