反应详情

To an acetic acid (10 mL) suspension of 1.07 g of 4-{3-[4-(3-{4-[amino(hydroxyimino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}-N′-hydroxybenzamidine was added 0.64 mL of acetic anhydride at room temperature, which was then stirred at room temperature for 40 minutes. To this mixture was added 0.10 g of 5% palladium-carbon, which was then stirred under hydrogen atmosphere for 2 hours and 15 minutes. Insoluble matter was filtered off before adding 4 mL of 6.0 mol/L hydrochloric acid, and insoluble matter was then filtered off, followed by distilling off the solvent under reduced pressure. A 5.0 mol/L sodium hydroxide aqueous solution was added to the resultant residue to adjust the pH to 12.5, followed by collecting the solid matter by filtration to provide 0.61 g of 4-{3-[4-(3-{4-[amino(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine as white solid form.

1. stirringwas then stirred under hydrogen atmosphere for 2 hours and 15 minutes
2. filtrationInsoluble matter was filtered off
3. additionbefore adding 4 mL of 6.0 mol/L hydrochloric acid, and insoluble matter
4. filtrationwas then filtered off
5. distillationby distilling off the solvent under reduced pressure
6. additionA 5.0 mol/L sodium hydroxide aqueous solution was added to the resultant residue
7. customby collecting the solid matter
8. filtrationby filtration