Hydrogen Peroxide → 1-(3-Hydroxypropyl)-5-hydroxymethylimidazole

HRID 987199

반응식

HRID 987199 반응식
[OH:1][CH2:2][CH2:3][CH2:4][N:5]1[C:9]([CH2:10][OH:11])=[CH:8][N:7]=[C:6]1S.OO.[OH-].[Na+]>CO.O.O[W](O)(=O)=O>[OH:1][CH2:2][CH2:3][CH2:4][N:5]1[C:9]([CH2:10][OH:11])=[CH:8][N:7]=[CH:6]1

참가 물질

7

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 1785208221-(3-Hydroxypropyl)-2-mercapto-5-hydroxymethylimidazole

생성물 1

HCID 229886421-(3-Hydroxypropyl)-5-hydroxymethylimidazole수율 95.6%

시약·촉매·용매 3

HCID 1152Tungstic acid촉매HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

1-(3-Hydroxypropyl)-2-mercapto-5-hydroxymethylimidazole(5.0 g, 23.1 mmol) and tungstic acid(H2WO4, 58 mg, 1 mol %) were mixed in 25 ml of methanol and 25 ml of distilled water. The mixture was warmed to 40° C. and 3.6 g of 30% hydrogen peroxide was added dropwise thereto. The whole mixture was stirred for 15 minutes and cooled and then, neutralized with 1 N sodium hydroxide solution. The resulting mixture was extracted twice with 25 ml of n-butanol and the solvent was distilled under reduced pressure to give 3.45 g(Yield 80.7%) of the title compound. 1H NMR (500 MHz, CDCl3) δ 7.46 (1H, s), 6.91 (1H, s), 4.61 (2H, s), 4.15 (2H, t, J=7 Hz), 3.52 (2H, t, J=7 Hz), 2.01 (2H, m).

후처리

  1. temperaturecooled
  2. extractionThe resulting mixture was extracted twice with 25 ml of n-butanol
  3. distillationthe solvent was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-8e9566bc6dcb4904b94cfead5e15585a
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630593B1

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