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Water → HCID 68701294、化合物

HRID 1988862
ノート
印刷プレビュー

反応式

HRID 1988862 の反応式
[CH2:1]([N:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:26]#N)[C:15]=2[O:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[C:10]([CH3:28])=[C:9]1[CH3:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-:30].[K+].[OH2:32]>C(O)C>[CH2:1]([N:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:26]([OH:32])=[O:30])[C:15]=2[O:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[C:10]([CH3:28])=[C:9]1[CH3:29])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物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 962Water2 回HCID 14797Potassium HydroxideHCID 68705257HCID 68705257、化合物

生成物 1

HCID 68701294HCID 68701294、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-Benzyl-7-(4-fluorobenzyloxy)-2,3-dimethyl-1H-pyrrolo[3,2-b]pyridine-6-carbonitrile (500 mg, 1.30 mmol) prepared in Example 276 was diluted with a mixture of ethanol (8 ml) and water (2 ml). Potassium hydroxide (650 mg, 13.0 mmol) was added to the solution, which was then refluxed for 24 hours. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The separated organic layer was dried on anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified with silica gel column chromatography (ethyl acetate/methanol=5/1, (v/v)) to give 280 mg of the titled compound as a white solid.

後処理

  1. temperaturewas then refluxed for 24 hours
  2. extractionwas then extracted with ethyl acetate
  3. dry with materialThe separated organic layer was dried on anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified with silica gel column chromatography (ethyl acetate/methanol=5/1, (v/v))

出典と根拠

ORDレコード
ord-1e6bb6737b024a109e6eb05630ac5abc
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07642269B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート