反应详情

温度

50 °C

Borane-dimethylsulfide complex (10M-THF solution; 5 ml) was added to a THF (20 ml) solution of 4-benzyl-N,N-dimethyl-3-oxo-3,4-dihydro-2-quinoxalinecarboxamide (1.5 g). The reaction mixture was stirred at room temperature for one hour, further at 50° C. for 18 hours, then concentrated. The residue was dissolved in methanol (30 ml) and the mixture was stirred at 50° C. for 20 hours together with 6N hydrochloric acid (10 ml). The reaction mixture was concentrated, and the residue was dissolved in pyridine (10 ml). Acetic anhydride (0.5 ml) was added to the reaction mixture, which was stirred at room temperature for 5 hours. The reaction mixture was concentrated, and the residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/3) to obtain the entitled compound (0.6 g).

1. concentrationconcentrated
2. dissolutionThe residue was dissolved in methanol (30 ml)
3. stirringthe mixture was stirred at 50° C. for 20 hours together with 6N hydrochloric acid (10 ml)
4. concentrationThe reaction mixture was concentrated
5. dissolutionthe residue was dissolved in pyridine (10 ml)
6. additionAcetic anhydride (0.5 ml) was added to the reaction mixture, which
7. stirringwas stirred at room temperature for 5 hours
8. concentrationThe reaction mixture was concentrated
9. customthe residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/3)