반응 #1147148

ord-111a1b45b6f54895952c275907f26941

반응 조건

온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with ethyl acetate
  2. 2
    세척The separated organic layer was washed with water and brine
  3. 3
    건조dried over sodium sulfate
  4. 4
    기타evaporated under reduced pressure
  5. 5
    기타The residue was triturated with diisopropyl ether
  6. 6
    여과filtered
  7. 7
    세척washed with diisopropyl ether
  8. 8
    기타dried under reduced pressure

실험 절차

To a suspension of 4-(4-methoxypyridin-2-yl)chlorobenzene (500 mg) in sulfuric acid (4 ml) was added fuming nitric acid (0.2 ml) dropwise at 0° C., and the mixture was stirred at 5° C. for 30 minutes. The reaction mixture was poured into a saturated aqueous sodium hydrogencarbonate solution and extracted with ethyl acetate. The separated organic layer was washed with water and brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was triturated with diisopropyl ether, filtered, washed with diisopropyl ether and dried under reduced pressure to give 1-chloro-4-(4-methoxypyridin-2-yl)-2-nitrobenzene (601 mg).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06521643B1uspto-grants-2003_02