反应详情

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

1. extractionlower, 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-butyl methyl ether
4. additionwas added to the resulting residue, and solids
5. filtrationwere filtered