反应详情

4-(Piperidin-4-yl)morpholin-3-one (0.18 g) obtained in Example 7c), (2S)-3[(6-chloronaphthalen-2-yl)sulfonyl]-2-hydroxypropionic acid (0.31 g) and HOBt (0.23 g) were dissolved in DMF (10 mL), WSC (0.29 g) was added thereto, and the mixture was stirred at room temperature for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with an aqueous sodium bicarbonate solution, and extracted with ethyl acetate. The extract was washed successively with water, an aqueous 5% citric acid solution, and saturated saline solution, and dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (form ethyl acetate to ethyl acetate/methanol=5/1) to obtain the title compound (0.20 g, 42%) as a colorless powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionthe residue was diluted with an aqueous sodium bicarbonate solution
3. extractionextracted with ethyl acetate
4. washThe extract was washed successively with water
5. dry with materialan aqueous 5% citric acid solution, and saturated saline solution, and dried over sodium sulfate
6. distillationthe solvent was distilled off under reduced pressure
7. customThe residue was purified by silica gel column chromatography (form ethyl acetate to ethyl acetate/methanol=5/1)