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Hydrogen Peroxide → HCID 54199337、化合物

HRID 1587709
ノート
印刷プレビュー

反応式

HRID 1587709 の反応式
[CH2:1]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[OH:18]O>C(O)(=O)C>[CH2:1]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][N+:13]=1[O-:18])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 784Hydrogen Peroxide2 回HCID 5646402-Undecylpyridine

生成物 1

HCID 54199337HCID 54199337、化合物収率 91%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 11.0 g (47 mmol) of 2-n-undecylpyridine and 8 ml of an aqueous 35% hydrogen peroxide dissolved in 30 ml of glacial acetic acid was heated at 70° to 80° C. for 3 hours, and further 3 ml of the aqueous hydrogen peroxide was added, followed by heating at the same temperature for 9 hours. After cooling, the mixture was concentrated under a reduced pressure to about a half amount, and 50 ml of water was added and the mixture concentrated to a half amount (repeated twice). The concentrate was extracted with diethyl ether and washed with an aqueous sodium hydrogen carbonate solution. The product was dried over anhydrous sodium sulfate and concentrated under a reduced pressure. The residue was purified by separation by silica gel column chromatography (ethyl acetate→methanol:ethyl acetate=15:85) to give 10.7 g of the desired product (yield 91.0%).

後処理

  1. temperaturewas heated at 70° to 80° C. for 3 hours
  2. temperatureby heating at the same temperature for 9 hours
  3. temperatureAfter cooling
  4. concentrationthe mixture was concentrated under a reduced pressure to about a half amount, and 50 ml of water
  5. additionwas added
  6. concentrationthe mixture concentrated to a half amount (
  7. extractionThe concentrate was extracted with diethyl ether
  8. washwashed with an aqueous sodium hydrogen carbonate solution
  9. dry with materialThe product was dried over anhydrous sodium sulfate
  10. concentrationconcentrated under a reduced pressure
  11. customThe residue was purified by separation by silica gel column chromatography (ethyl acetate→methanol:ethyl acetate=15:85)

出典と根拠

ORDレコード
ord-85dfa946f33d4e1b8d13af6e1d22b804
出典データセット
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05219847

反応ノート

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