반응 #345439

ord-89091551cdc042e1b4eaf81ecb2d4369

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After completion of the reaction
  2. 2
    추출extracted with ethyl acetate
  3. 3
    세척The extract was washed
  4. 4
    건조dried over magnesium sulfate
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타The residue was purified by silica gel column chromatography with hexane-ethyl acetate (4:1)

실험 절차

To a solution of 5-(3-chloro-5-trifluoromethylpyridin-2-yl)[1,2,3]triazolo[4,5-f]indazole [Compound No. 48] (1.0 g) in N,N-dimethylformamide (10 g), methyl 2-bromopropionate (0.5 g) and potassium carbonate (1 g) were added, and the resultant mixture was stirred at 40° C. for 3 hours. After completion of the reaction, the reaction mixture was poured into water and extracted with ethyl acetate. The extract was washed, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography with hexane-ethyl acetate (4:1) to give 5-(3-chloro-5-trifluoromethylpyridin-2-yl)-3-(1-methoxycarbonylethyl)[1,2,3]triazolo[4,5-f]indazole (0.3 g) and 5-(3-chloro-5-trifluoromethylpyridin-2-yl)-1-(1-methoxycarbonylethyl)[1,2,3]triazolo[4,5-f]indazole (0.1 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05266556uspto-grants-1993_11