반응 #966166

ord-5734440650dc40a4b18216a4247e11e4

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture was heated
  2. 2
    온도at reflux for 16 hours
  3. 3
    농축The reaction mixture was concentrated under reduced pressure
  4. 4
    추출extracted with ethyl acetate
  5. 5
    건조The obtained organic layer was dried over anhydrous sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축the filtrate was concentrated under reduced pressure

실험 절차

To a solution of 4-Methyl-3-nitrobenzoic acid (25.4 g) in methanol (300 mL) was slowly added concentrated sulfuric acid (2 mL), and then the reaction mixture was heated at reflux for 16 hours. The reaction mixture was concentrated under reduced pressure, and then the reaction mixture was neutralized with a saturated aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure to give the titled compound (26.9 g) as a pale yellow solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08987473B2uspto-grants-2015_03