反应详情

To a solution of 2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]pyridine-3-carbaldehyde (0.210 g, 0.438 mmol) in ethanol (3 mL) are added hydroxylamine hydrochloride (0.038 g, 0.526 mmol) and sodium ethanoate (0.044 g, 0.526 mmol) and the mixture is stirred at reflux for 1 h. The solvent is evaporated and the residue is extracted with ethyl acetate and water. The organic layer is separated, dried over magnesium sulfate, filtered and the solvent is evaporated in vacuo. The residue is purified by basic reverse phase HPLC to yield 0.110 g of 2-[4-[(2-chloro-4,4-difluoro-spiro[5H-thieno[2,3-c]pyran-7,4′-piperidine]-1′-yl)methyl]-3-methyl-pyrazol-1-yl]pyridine-3-carbaldehyde oxime. MS (m/z): 494 (M+1).

1. temperatureat reflux for 1 h
2. customThe solvent is evaporated
3. extractionthe residue is extracted with ethyl acetate and water
4. customThe organic layer is separated
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent is evaporated in vacuo
8. customThe residue is purified by basic reverse phase HPLC