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Hydrogen Peroxide → Pyridine, 3-ethyl-, 1-oxide

HRID 1913756
ノート
印刷プレビュー

反応式

HRID 1913756 の反応式
[CH2:1]([C:3]1[CH:4]=[N:5][CH:6]=[CH:7][CH:8]=1)[CH3:2].OO.C(=O)([O-])[O-:12].[Na+].[Na+]>C(O)(=O)C>[CH2:1]([C:3]1[CH:4]=[N+:5]([O-:12])[CH:6]=[CH:7][CH:8]=1)[CH3:2]
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 784Hydrogen Peroxide2 回HCID 10340Sodium CarbonateHCID 108233-Ethylpyridine

生成物 1

HCID 84685Pyridine, 3-ethyl-, 1-oxide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

A mixture of 10.0 g of 3-ethylpyridine, 60 ml of acetic acid and 12 ml of 30% hydrogen peroxide solution was stirred while heating at 80° C. for 2.5 hours. To the reaction mixture, 7 ml of 30% hydrogen peroxide solution was added, and the reaction mixture was stirred while heating at 80° C. for further seven hours. The reaction mixture was cooled to room temperature, and sodium carbonate was added to the reaction mixture in small portions. The reaction mixture was filtered, and washed with ethyl acetate. The resultant filtrate was washed with a saturated aqueous solution of sodium hydrogensulfite and a saturated sodium chloride solution, dried over anhydrous water sodium carbonate. Activated carbon was added, followed by filtration through Celite™. The filtrate was concentrated under reduced pressure to give 6.0 g of 3-ethylpyridine N-oxide.

後処理

  1. stirringthe reaction mixture was stirred
  2. temperaturewhile heating at 80° C. for further seven hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. filtrationThe reaction mixture was filtered
  5. washwashed with ethyl acetate
  6. washThe resultant filtrate was washed with a saturated aqueous solution of sodium hydrogensulfite
  7. dry with materiala saturated sodium chloride solution, dried over anhydrous water sodium carbonate
  8. additionActivated carbon was added
  9. filtrationfollowed by filtration through Celite™
  10. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-1b014344b2004d42b29526779c1bbf68
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609705B2

反応ノート

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