反应详情

To an N,N-dimethylformamide (10 mL) suspension of 1.00 g of 4-{3-[4-(3-{4-[amino(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine was added 4-nitrophenyl=acetate at room temperature, which was then stirred at the same temperature for 1 hour and 15 minutes. Chloroform and a 5% potassium carbonate aqueous solution were added to the reaction mixture, and insoluble matter was filtered off. The organic layer was separated, washed sequentially with a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution, and then dried with anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure. Ethyl acetate and water were added to the resultant residue, which was then adjusted to pH 3.0 using hydrochloric acid. The aqueous layer was separated and washed with ethyl acetate, which was then adjusted to pH 12.0 using a sodium hydroxide aqueous solution. The precipitate was collected by filtration to provide 0.80 g of N′-acetyl-4-{3-[4-(3-{4-[(acetylimino)(amino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine as white solid form.

1. filtrationwas filtered off
2. customThe organic layer was separated
3. washwashed sequentially with a 5% potassium carbonate aqueous solution
4. dry with materiala saturated sodium chloride aqueous solution, and then dried with anhydrous magnesium sulfate
5. distillationby distilling off the solvent under reduced pressure
6. additionEthyl acetate and water were added to the resultant residue, which
7. customThe aqueous layer was separated
8. washwashed with ethyl acetate, which
9. filtrationThe precipitate was collected by filtration