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Water → 3-(3-fluorophenyl)-1H-pyrazolo[4,3-b]pyridine

HRID 34000
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인쇄 미리보기

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HRID 34000 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]([C:10]2[C:15](F)=[CH:14][CH:13]=[CH:12][N:11]=2)=O)[CH:5]=[CH:6][CH:7]=1.O.[NH2:18][NH2:19].O>CO>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[C:10]3=[N:11][CH:12]=[CH:13][CH:14]=[C:15]3[NH:19][N:18]=2)[CH:5]=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 23070169(3-Fluorophenyl)-(3-fluoropyridin-2-yl)-methanone

생성물 1

HCID 100134493-(3-fluorophenyl)-1H-pyrazolo[4,3-b]pyridine

시약·촉매·용매 1

HCID 887Methanol용매

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온도
80 °C

실험 절차

1.5 g of (3-fluorophenyl)-(3-fluoropyridin-2-yl)-methanone was dissolved in 5 mL of methanol, added with 1.0 mL of hydrazine monohydrate, and heated at 80° C. for 4 hours. The reaction solution was added with water, and extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:4), to afford 240 mg of the title compound as a colorless powder.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed successively with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off
  5. customthe residue was purified
  6. customseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:4)

출처 및 근거

ORD 기록
ord-ab132e1377fb4a9390315de1c1e71b20
출처 데이터셋
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07429609B2

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