反应详情

In chloroform (10 ml), 5-t-butoxycarbonylamino valeric acid (574 mg), WSCI hydrochloride (690 mg), and HOBt (487 mg) were dissolved. Then, the solution was stirred at room temperature for 30 minutes. The solution was added with the compound (503 mg) obtained in Example 3-1 and stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was then dissolved in chloroform. After having been washed with a saturated aqueous sodium hydrogen carbonate solution, a saturated aqueous ammonium chloride solution, and a saturated saline solution, the resultant was dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure and the residue was then purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (540 mg) as a colorless viscous substance.

1. stirringstirred overnight at room temperature
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. dissolutionthe residue was then dissolved in chloroform
5. washAfter having been washed with a saturated aqueous sodium hydrogen carbonate solution
6. dry with materiala saturated aqueous ammonium chloride solution, and a saturated saline solution, the resultant was dried with anhydrous sodium sulfate
7. filtrationAfter filtration
8. distillationthe solvent was distilled off under reduced pressure
9. customthe residue was then purified through silica gel column chromatography (chloroform/ethyl acetate)