反应详情

In chloroform/DMF (60 ml/30 ml), t-butoxycarbonylamino valeric acid (3.91 g), WSCI hydrochloride (4.02 g), and HOBt (2.82 g) were dissolved and the whole was stirred for 1 hour. The solution was added with the compound (2.32 g) obtained in Example 39-2 and the whole was stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform, washed with a saturated aqueous ammonium chloride solution, a saturated aqueous sodium hydrogen carbonate solution, and a saturated saline solution, and then dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (4.06 g) as a white solid.

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