反应详情

In chloroform (31 ml), 5-t-butoxycarbonylamino valeric acid (1.57 g), WSCI hydrochloride (1.98 g), and HOBt (1.39 g) were dissolved. Then, the solution was stirred at room temperature for 30 minutes. The solution was dropped in a chloroform solution (10 ml) containing the compound (1.18 g) obtained in Example 5-2. Then, the whole was stirred at room temperature for 12 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform and then washed with a saturated aqueous sodium hydrogen carbonate solution, a saturated aqueous ammonium chloride solution, and a saturated saline solution, followed by drying 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) to remove only highly-polar components, thereby obtaining a mixture (2.52 g) containing the subject compound as a yellow oily substance.

1. stirringThen, the whole was stirred at room temperature for 12 hours
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 sodium hydrogen carbonate solution
6. dry with materialby drying 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)
10. customto remove only highly-polar components