反应详情

In a small amount of a saturated aqueous solution of potassium carbonate was dissolved β-alanine t-butyl ester hydrochloride (1.5 g), followed by extraction with methylene chloride. The extract was dried and concentrated into 720 mg of β-alanine t-butyl ester in the free form. The resulting ester and a 1,4-dioxane (2.0 ml) solution of the 2,5-dichloro-4-[(4-chlorophenylthio)-(2,5-difluorophenyl)methyl]pyridine (300 mg, 0.72 mmol) obtained in Example 54 was stirred at 120° C. for 4 days under an argon atmosphere. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate. The diluted mixture was washed with water and brine, dried and then concentrated under reduced pressure. The residue thus obtained was purified by silica gel chromatography (hexane:ethyl acetate=5:1) to give the title compound (79 mg, 16%) as an oil.

1. extractionfollowed by extraction with methylene chloride
2. customThe extract was dried
3. concentrationconcentrated into 720 mg of β-alanine t-butyl ester in the free form
4. washThe diluted mixture was washed with water and brine
5. customdried
6. concentrationconcentrated under reduced pressure
7. customThe residue thus obtained
8. customwas purified by silica gel chromatography (hexane:ethyl acetate=5:1)