反应详情

Compound 1a (9.69 g, 21.9 mmol) was dissolved in 200 mL of methanol, to which 500 mg of 10% palladium carbon was then added, followed by stirring at room temperature for one day under an atmosphere of hydrogen. The catalyst was filtered off from the reaction mixture, followed by concentration under reduced pressure. This residue, Cbz-Phe (6.92 g, 23.1 mmol), HOBT (3.71 g, 24.2 mmol), and NMM (2.66 mL, 24.2 mmol) were dissolved in 50 mL of dimethylformamide (DMF), to which EDC (4.64 g, 24.2 mmol) was then added under stirring and cooling with ice, followed by stirring at room temperature for one day. Water was added to the reaction solution, which was then washed with a 10% citric acid aqueous solution, a saturated sodium bicarbonate solution, and water before drying. The resultant residue was purified using silica gel column chromatography (elution solvent: chloroform:methanol=90:10) to provide 12.8 g of the title compound as a white solid.

1. additionwas then added
2. filtrationThe catalyst was filtered off from the reaction mixture
3. concentrationfollowed by concentration under reduced pressure
4. additionwas then added
5. stirringunder stirring
6. temperaturecooling with ice
7. stirringby stirring at room temperature for one day
8. washwas then washed with a 10% citric acid aqueous solution
9. dry with materiala saturated sodium bicarbonate solution, and water before drying
10. customThe resultant residue was purified
11. washsilica gel column chromatography (elution solvent: chloroform:methanol=90:10)