反应详情

To a solution of Boc-D-tert-leucine (0.23 g) and HOBt (0.23 g) in acetonitrile (5 ml) was added WSC (0.29 g), and the reaction mixture was mixed at room temperature for 15 minutes. Then, a solution of 5-methyl-2-(4-piperidinyl)-1,2-dihydro-3H-imidazo[1,5-c]imidazol-3-one dihydrochloride (0.29 g), DBU (0.30 g) and triethylamine (0.30 g) in acetonitrile (5 ml) was added thereto. The reaction mixture was mixed at room temperature for 15 hours, the solvent was then distilled off under reduced pressure, and the residue was dissolved in ethyl acetate. The ethyl acetate solution was washed with an aqueous sodium hydrogen carbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified with basic silica gel column (ethyl acetate to ethyl acetate/methanol=5/1) to obtain the title compound as colorless powder (0.40 g, 92%).

1. additionthe reaction mixture was mixed at room temperature for 15 minutes
2. additionThe reaction mixture was mixed at room temperature for 15 hours
3. distillationthe solvent was then distilled off under reduced pressure
4. dissolutionthe residue was dissolved in ethyl acetate
5. washThe ethyl acetate solution was washed with an aqueous sodium hydrogen carbonate solution
6. dry with materialdried over anhydrous sodium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. customthe residue was purified with basic silica gel column (ethyl acetate to ethyl acetate/methanol=5/1)