反应详情

A solution of 1-((6-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidin-2-yl)methyl)-3-(trifluoromethyl)-1H-pyrazole-4-carbaldehyde (2.92 mmol, 1 g) and hydroxylamine hydrochloride (3.21 mmol, 0.223 g) in ethanol (7 mL) was heated to 80° C. and this temperature was maintained for 3 h. The reaction mixture was allowed to cool to room temperature & diluted with ether and heptane before the resulting precipitate was collected by filtration. The resulting solid was taken up in acetic acid (5 mL) and zinc (7.79 mmol, 0.510 g) and the whole was stirred at room temperature for 3 days with occassional agitation by sonication. The reaction mixture was filtered through celite and the pad washed with MeOH before the filtrate was concentrated under reduced pressure. The residue was dissolved in MeOH and applied to an SCX cartridge that had been equilibrated with the same solvent before being eluted with 2N NH3/MeOH to give a light yellow solid (271 mg, 0.79 mmol, 50.6%)

1. temperaturethis temperature was maintained for 3 h
2. filtrationwas collected by filtration
3. filtrationThe reaction mixture was filtered through celite
4. washthe pad washed with MeOH before the filtrate
5. concentrationwas concentrated under reduced pressure
6. dissolutionThe residue was dissolved in MeOH
7. washbefore being eluted with 2N NH3/MeOH