反应详情

To a dichloromethane (120 mL) solution of di-tert-butyl (3-(3-(4-((pyridin-2-yloxy)methyl)benzyl)isoxazol-5-yl)pyridin-2-yl)imidodicarbonate (11.8 g, purity about 70%) described in Manufacturing Example 1-4-2 was added trifluoracetic acid (40 mL) at 0° C., which was stirred at room temperature for 14 hours. To the reaction mixture was added saturated aqueous sodium bicarbonate at 20° C. or less, which was then extracted with ethyl acetate and purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1). The solvent was concentrated under a reduced pressure, tert-butylmethyl ether was added to the resulting residue, and the solids were filtered to obtain the title compound (7.29 g).

1. extractionwhich was then extracted with ethyl acetate
2. custompurified by NH silica gel column chromatography (heptane:ethyl acetate=1:1)
3. concentrationThe solvent was concentrated under a reduced pressure, tert-butylmethyl ether
4. additionwas added to the resulting residue
5. filtrationthe solids were filtered