반응 #41782

ord-1b337a0935334edbab9388c479de6e9a

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGstirred overnight at 60° C
  2. 2
    온도The reaction was cooled down to room temperature
  3. 3
    기타evaporated
  4. 4
    세척washed with water and brine
  5. 5
    기타dried
  6. 6
    기타evaporated under reduced pressure

실험 절차

A solution of the methyl5-[3-amino-4-(methylamino)phenoxy]pyridine-3-carboxylate (1 eq) in methanol (8 ml) was treated with 4-bromophenylisothiocyanate (1 eq) and stirred at 60° C.-65° C. for 2 hours. The reaction mixture was cooled down to room temperature and methyl iodide (1 eq) was added and stirred overnight at 60° C. The reaction was cooled down to room temperature, evaporated, taken up in ethyl acetate and washed with water and brine, dried, evaporated under reduced pressure. Column chromatography yielded methyl5-{2-[(4-bromophenyl)amino]-1-methylbenzimidazol-5-yloxy}pyridine-3-carboxylate. MS: MH+=452

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728010B2uspto-grants-2010_06