反应详情

温度

60 °C

To a solution of 4-[4-(bromomethyl)benzenesulfonyl]-1-[1-(tert-butoxycarbonyl)-4-piperidylmethyl]-2-piperazinone (2.85 g) in DMF (30 ml) was added potassium acetate (1.58 g), and the mixture was stirred at 60° C. for 4 hours. The reaction solution was concentrated under reduced pressure, and to the residue was added ethyl acetate. The mixture was washed with water and saturated brine, dried and concentrated, and the residue was dissolved in methanol (50 ml). To the solution was added sodium methoxide (28% methanol solution, 290 mg), and the mixture was stirred at room temperature for 2 hours. The reaction solution was concentrated under reduced pressure, and to the residue was added ethyl acetate. The mixture was washed with water and saturated brine, dried (MgSO4) and concentrated. The residual crystals were washed with ether to give colorless crystals of 1-[1-(tert-butoxycarbonyl)-4-piperidylmethyl]-4-[4-(hydroxymethyl)benzenesulfonyl]-2-piperazinone (2.02 g).

1. concentrationThe reaction solution was concentrated under reduced pressure
2. additionto the residue was added ethyl acetate
3. washThe mixture was washed with water and saturated brine
4. customdried
5. concentrationconcentrated
6. dissolutionthe residue was dissolved in methanol (50 ml)
7. additionTo the solution was added sodium methoxide (28% methanol solution, 290 mg)
8. stirringthe mixture was stirred at room temperature for 2 hours
9. concentrationThe reaction solution was concentrated under reduced pressure
10. additionto the residue was added ethyl acetate
11. washThe mixture was washed with water and saturated brine
12. dry with materialdried (MgSO4)
13. concentrationconcentrated
14. washThe residual crystals were washed with ether