Sodium Hydroxide → 5H-Indeno(1,2-b)pyridin-5-one

HRID 1093029

反応式

HRID 1093029 の反応式
[OH-].[Na+].[N:3]1[C:16]2[C:7](=C3[C:13](=[CH:14][CH:15]=2)[CH:12]=[CH:11][C:10](=O)[C:9]3=[O:18])[CH:6]=[CH:5][CH:4]=1>>[CH:6]1[C:7]2[C:9](=[O:18])[C:10]3[C:15](=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:16]=2[N:3]=[CH:4][CH:5]=1

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 199224561-Azaphenanthrene-5,6-dione

生成物 1

HCID 774895H-Indeno(1,2-b)pyridin-5-one収率 38%

反応条件

温度
85 °C

実験手順

Subsequently, in a stream of argon, 1.5 L of a 10% aqueous solution of sodium hydroxide was added to 51.0 g (244 mmol) of 1-azaphenanthrene-5,6-dione, and heated and stirred at 85° C. for 90 minutes. After the mixture was cooled to room temperature, the precipitate was filtered out. The filtrate was extracted with chloroform and concentrated, and added to the precipitate, whereby a crude material was obtained. The crude material was purified by chromatography on silica gel with toluene/ethyl acetate=10:1 to give 16.8 g of 4-azafluorene-9-one (37.9% yield).

後処理

  1. temperatureheated
  2. temperatureAfter the mixture was cooled to room temperature
  3. filtrationthe precipitate was filtered out
  4. extractionThe filtrate was extracted with chloroform
  5. concentrationconcentrated
  6. additionadded to the precipitate, whereby a crude material
  7. customwas obtained
  8. customThe crude material was purified by chromatography on silica gel with toluene/ethyl acetate=10:1

出典と根拠

ORDレコード
ord-6a7b1117398e4e65b484f3b7d4a81c71
出典データセット
uspto-grants-2012_03
特許番号
US08129899B1

関連ノート

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