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

HRID 2094810

반응식

HRID 2094810 반응식
[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

참가 물질

4

반응물 2

HCID 784Hydrogen PeroxideHCID 788945-Ethyl-2-pyridineethanol

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8dc1f5f2c6134959ae98cd70b25b1595
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445685B2

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