反应详情

To a solution of 2-{6-[({[(1-methyl-1H-imidazol-5-yl)(3-thienyl)methylene]amino}oxy)-methyl]pyridin-2-yl}-1H-isoindole-1,3(2H)-dione (6.80 g, 15.3 mmol) in tetrahydrofuran (30 mL) was added dropwise hydrazine hydrate (3.72 mL, 76.7 mmol). After stirring at room temperature for 30 h, the reaction mixture was filtered, the insolubles washed with ethyl acetate, and the filtrate concentrated in vacuo. Purification on silica gel afforded 6-[({[(1-methyl-1H-imidazol-5-yl)(3-thienyl)methylene]amino}oxy)methyl]pyridin-2-amine [3.02 g, yield 60%; HPLC/MS: m/z=314 (M+H); log P(HCOOH)=0.39].

1. filtrationthe reaction mixture was filtered
2. washthe insolubles washed with ethyl acetate
3. concentrationthe filtrate concentrated in vacuo
4. customPurification on silica gel