반응 #423619

ord-f2cf162be07445fc8c94bb6e87175ec1

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After completion of the reaction
  2. 2
    여과the reaction mixture was filtered through a cellite
  3. 3
    세척washed with methanol
  4. 4
    농축concentrated under reduced pressure
  5. 5
    기타The solid thus obtained
  6. 6
    여과was filtered
  7. 7
    세척washed with ether
  8. 8
    기타dried

실험 절차

4-(Pyridin-3-yl)oxy-1-nitrobenzene prepared in Step A was dissolved in the mixture of water (100 mL), tetrahydrofuran (100 mL) and methanol (100 mL). Iron powder (103 g, 1.84 mol) and ammonium chloride (99 g, 1.84 mol) were added thereto, and the mixture was stirred for 3 h at 80° C. using a mechanical stirrer. After completion of the reaction, the reaction mixture was filtered through a cellite, washed with methanol, and concentrated under reduced pressure. The solid thus obtained was filtered, washed with ether, and dried to give the title compound (17 g, Yield 36%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08889691B2uspto-grants-2014_11