反应 #1831047
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08435995B2
反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 3-[3-(dimethylamino)prop-2-enoyl]-1-[3-(trifluoromethyl)phenyl]pyridazin-4(1H)-one (500 mg, 1.5 mmol) in ethanol (10 mL) were added 2-methylpropylhydrazine hydrochloride (274 mg, 2.2 mmol) and Et3N (0.41 mL, 3.0 mmol). The mixture was stirred at 100° C. for 5 h. The mixture was diluted with 1N HCl aqueous solution, extracted with AcOEt, washed with brine, dried over Na2SO4, concentrated in vacuo, purified by column chromatography on silica gel (hexane/AcOEt=10/90 to 0/100) and recrystallized with AcOEt/i-Pr2O to yield the title compound as a pale yellow solid (289 mg, 54%). extracted with AcOEt washed with brine dried over Na2SO4 concentrated in vacuo purified by column chromatography on silica gel (hexane/AcOEt=10/90 to 0/100) recrystallized with AcOEt/i-Pr2O
来源 ID: ord-a9aedda8079a4995bd9f6a9ce1d1e62f