反应 #3573784
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05646283
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Potassium hydroxide (790 mg, 12.0 mmol) was dissolved in 3 ml of water, and 400 mg (2.40 mmol) of 5-fluoroisatin was added thereto. To this was added 600 mg (2.40 mmol) of compound s obtained in Reference Example 19 which was dissolved in dioxane-ethanol (2 ml-4 ml). The mixture was heat-refluxed for 6 days. The solvent was distilled off, and the residue was dissolved in water and washed with ether. The aqueous layer was filtered through Celite, and acetic acid was added to the flitrate. The precipitated crystals were collected by filtration. These crystals were then dried under reduced pressure, and recrystallized from dimethylformamide-water to obtain 460 mg of the above-mentioned compound (yield 48%). obtained in Reference Example 19 which The mixture was heat-refluxed for 6 days The solvent was distilled off the residue was dissolved in water washed with ether The aqueous layer was filtered through Celite, and acetic acid was added to the flitrate The precipitated crystals were collected by filtration These crystals were then dried under reduced pressure recrystallized from dimethylformamide-water
来源 ID: ord-ef5395167b814c01b887325808a1247e