反应详情

温度

65 °C

The 5-chloro-4-[(4-chlorophenylsulfonyl)(2,6-difluorophenyl)methyl]-2-(3,4-dimethoxybenzylamino)pyridine (293 mg, 0.506 mmol) obtained in Example 295 was dissolved in trifluoroacetic acid (4 ml). The resulting solution was heated at 65° C. for 2 hours. The reaction mixture was concentrated. The residue thus obtained was basified with a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate. The extract was washed with water and brine, dried over magnesium sulfate, and concentrated. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the hexane:ethyl acetate=2:1 eluate was concentrated. The solid thus obtained was recrystallized from ethyl acetate-hexane to give the title compound (147 mg, 0.343 mmol, 68%) as a white solid.

1. concentrationThe reaction mixture was concentrated
2. customThe residue thus obtained
3. extractionfollowed by extraction with ethyl acetate
4. washThe extract was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated
7. customThe residue thus obtained
8. concentrationethyl acetate=2:1 eluate was concentrated
9. customThe solid thus obtained
10. customwas recrystallized from ethyl acetate-hexane