반응 #59075

ord-b877ca9cf4694fe29ed1e742856a09bc

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The reaction mixture was then concentrated
  2. 2
    기타partitioned between ethyl acetate and water
  3. 3
    기타The organic layer was separated
  4. 4
    세척washed with water
  5. 5
    건조brine, dried over sodium sulfate
  6. 6
    농축concentrated
  7. 7
    기타to give orange solid
  8. 8
    기타Purification on silica gel with 20% methanol in methylene chloride

실험 절차

The mixture containing N-(4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-yl)-2-chloroacetamide (1 eq), 1-ethylpiperazine (3 eq), and potassium carbonate (4 eq) was stirred in dimethylformamide at 60° C. for 1 hour. The reaction mixture was then concentrated and partitioned between ethyl acetate and water. The organic layer was separated and washed with water then brine, dried over sodium sulfate and concentrated to give orange solid. Purification on silica gel with 20% methanol in methylene chloride gave N-(4-(4-(methylamino)-3-nitrophenoxy)pyridin-2-yl)-2-(4-ethylpiperazin-1-yl)acetamide as a red solid. HPLC=3.26 min; MS: MH+=415.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07423150B2uspto-grants-2008_09