反応 #41781

ord-bf6dc933770b47d2a8ca9040f0f8e650

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他evaporated
  2. 2
    洗浄washed with water, brine
  3. 3
    その他dried
  4. 4
    その他evaporated
  5. 5
    その他The crude was purified by column chromatography

実験手順

To the solution of the methyl5-[3-nitro-4-(2,2,2-trifluoroacetylamino)phenoxy]-pyridine-3-carboxylate (1 eq) in a mixture of toluene, acetonitrile and sodium hydroxide solution (50%) was added benzyltrimethylammonium chloride (1 eq) and dimethyl sulfate (1.2 eq). The biphasic mixture was stirred overnight at room temperature and evaporated. The mixture was taken up in ethyl acetate, washed with water, brine, dried and evaporated. The crude was purified by column chromatography to afford methyl-4-[4-(methylamino)-3-nitrophenoxy]pyridine-3-carboxylate. MS: MH+=303.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07728010B2uspto-grants-2010_06