반응 #95677

ord-87a3a592b65443759832102a9c1a8ecf

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타(ca 2.5 hours)
  2. 2
    온도After cooling
  3. 3
    기타removal of the unreacted 6-fluoro-2-nitrotoluene
  4. 4
    추출by extraction with ethyl acetate
  5. 5
    추출extracted three times with ethyl acetate
  6. 6
    건조The combined organic extracts are dried over magnesium sulphate
  7. 7
    농축concentrated

실험 절차

A mixture of 34.5 g (0.22 mol) of 6-fluoro-2-nitrotoluene, 30.7 g (0.22 mol) of potassium carbonate, 105.4 g (0.66 mol) of potassium permanganate and 3.3 liters of water is heated at 100° C. until the permanganate is decolorised (ca 2.5 hours). After cooling and removal of the unreacted 6-fluoro-2-nitrotoluene by extraction with ethyl acetate, the aqueous phase is adjusted to pH 1 with hydrochloric acid and extracted three times with ethyl acetate. The combined organic extracts are dried over magnesium sulphate and concentrated, there being obtained 6-fluoro-2-nitrobenzoic acid. After recrystallisation from ethyl acetate/n-hexane, the product melts at 146°-148° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04346032uspto-grants-1982_08