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

HRID 34000
ノート
印刷プレビュー

反応式

HRID 34000 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-ab132e1377fb4a9390315de1c1e71b20
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07429609B2

反応ノート

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