反应详情

温度

32.5 °C

To 9 mL of an ethanol solution containing 0.16 g of 7-methoxy-1-(2-(4-oxocyclohexyl)ethyl)quinoxalin-2(1H)-one, 54 mg of ammonium acetate and 0.32 g of molecular sieves 3A were added at room temperature, and the mixture was stirred in an external bath at 30 to 35° C. for 1 hour and 30 minutes. The reaction mixture was cooled to room temperature, 35 mg of sodium cyanoborohydride was added thereto, and the mixture was stirred for 15 minutes. The reaction mixture was added with water and ethyl acetate, and the resultant solution was adjusted to pH 5.2 with 2.0 mol/L hydrochloric acid, and the aqueous layer was separated. The aqueous layer was added with ethyl acetate, and the resultant solution was adjusted to pH 9.5 with an aqueous sodium hydrogen carbonate solution. The organic layer was separated, and the aqueous layer was extracted sequentially with ethyl acetate and chloroform. The organic layer and the extract were combined, the resultant solution was dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure to obtain 60 mg of a yellow oily substance, 1-(2-(4-aminocyclohexyl)ethyl)-7-methoxyquinoxalin-2(1H)-one.

1. additionwere added at room temperature
2. temperatureThe reaction mixture was cooled to room temperature
3. stirringthe mixture was stirred for 15 minutes
4. customthe aqueous layer was separated
5. additionThe aqueous layer was added with ethyl acetate
6. customThe organic layer was separated
7. extractionthe aqueous layer was extracted sequentially with ethyl acetate and chloroform
8. dry with materialthe resultant solution was dried over anhydrous magnesium sulfate
9. customthe solvent was removed under reduced pressure