反应详情

Into a suspension of 1.07 g of 4-{3-[4-(3-{4-[amino(hydroxyimino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}-N′-hydroxybenzamidine in 10 mL of acetic acid, 0.64 mL of acetic anhydride was added at room temperature, and the suspension was stirred at room temperature for 40 min. The mixture, after adding 0.10 g of 5% palladium on carbon, was stirred under hydrogen atmosphere for 2 hours 15 min. The mixture was filtered to remove insoluble matters, and after adding 4 mL of 6.0 mol/L hydrochloric acid, the mixture was filtered again to remove insoluble matters, and the solvent was removed by evaporation under reduced pressure. To the obtained residue, a 5.0 mol/L sodium hydroxide aqueous solution was added to adjust the pH to 12.5, then the solid matter was collected by filtration to obtain 0.61 g of 4-{3-[4-(3-{4-[amino(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine as a white solid.

1. additionwas added at room temperature
2. stirringwas stirred under hydrogen atmosphere for 2 hours 15 min
3. filtrationThe mixture was filtered
4. customto remove insoluble matters
5. additionafter adding 4 mL of 6.0 mol/L hydrochloric acid
6. filtrationthe mixture was filtered again
7. customto remove insoluble matters
8. customthe solvent was removed by evaporation under reduced pressure
9. additionTo the obtained residue, a 5.0 mol/L sodium hydroxide aqueous solution was added
10. filtrationthe solid matter was collected by filtration