Hydrogen Peroxide → 2-(5-Ethyl-1-oxidopyridin-1-ium-2-yl)ethanol

HRID 2094810ノート

反応式

HRID 2094810 の反応式
[CH2:1]([C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][OH:11])=[N:7][CH:8]=1)[CH3:2].[OH:12]O>C(O)(=O)C>[CH3:2][CH2:1][C:3]1[CH:4]=[CH:5][C:6]([CH2:9][CH2:10][OH:11])=[N+:7]([O-:12])[CH:8]=1

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 788945-Ethyl-2-pyridineethanol

生成物 1

HCID 668233992-(5-Ethyl-1-oxidopyridin-1-ium-2-yl)ethanol収率 81.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
100 °C

実験手順

To a solution of 100 g (0.655 mol) 2-(5-ethyl-pyridin-2-yl)-ethanol in 500 mL acetic acid was added 118 g (1.049 mol) 30% hydrogen peroxide at 25-30° C. Reaction mixture was refluxed at 100° C. (tlc) for 14 hr. After completion of the reaction acetic acid was removed under vacuum, and the residual mass was poured in excess water and made alkaline by 10% Na2CO3 solution. Product was extracted with ethyl acetate and after concentrating ethyl acetate in vacuo, 89.58 g (81%) crystalline product was obtained.

後処理

  1. customReaction mixture
  2. customwas removed under vacuum
  3. additionthe residual mass was poured in excess water
  4. extractionProduct was extracted with ethyl acetate
  5. concentrationafter concentrating ethyl acetate in vacuo

出典と根拠

ORDレコード
ord-8dc1f5f2c6134959ae98cd70b25b1595
出典データセット
uspto-grants-2013_05
特許番号
US08445685B2

反応ノート

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