反应 #104152
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08536168B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Furan-2,3-dicarboxylic acid dimethyl ester (1.6 g, 8.69 mmol) is added to EtOH (10 mL) and hydrazine hydrate (1.46 mL, 55% in water). Heat the reaction to reflux for 5-6 h. Cool and concentrate in vacuo to form a slurry. Dilute the material with additional H2O and filter the precipitate. Wash with additional H2O. Transfer material from filter to a round bottom flask and add HCl (7.2 mL, 2N in H2O). Heat reaction mixture to reflux for 4 h. Cool and filter the precipitate washing with H2O, to yield the title compound without further purification (930 mg, 70%) Heat the reaction to reflux for 5-6 h Cool concentrate in vacuo to form a slurry filter the precipitate Wash with additional H2O Transfer material from filter to a round bottom flask add HCl (7.2 mL, 2N in H2O) Heat reaction mixture to reflux for 4 h Cool filter the precipitate washing with H2O
来源 ID: ord-2ebb0da334174606947c849ab3b2fdde