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Nitric Acid → (1-propyl-1H-imidazol-5-yl)methanol

HRID 1182366
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HRID 1182366 반응식
[N+]([O-])(O)=O.N([O-])=O.[Na+].[OH:9][CH2:10][C:11]1[N:15]([CH2:16][CH2:17][CH3:18])[C:14](S)=[N:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>O>[OH:9][CH2:10][C:11]1[N:15]([CH2:16][CH2:17][CH3:18])[CH:14]=[N:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 944Nitric AcidHCID 11430Potassium CarbonateHCID 23668193Sodium NitriteHCID 178456417(2-mercapto-1-propyl-1H-imidazol-5-yl)methanol

생성물 1

HCID 22938539(1-propyl-1H-imidazol-5-yl)methanol수율 58.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 5.0 M nitric acid (370 ml) was added sodium nitrite (1.14 g), and then 5-hydroxymethyl-2-mercapto-1-propylimidazole (71.0 g) was portionwise added at 0° C. The mixture was returned to room temperature and stirred for 2 hours, followed by adding water (200 ml). Thereto was added potassium carbonate at 0° C. to neutralize the mixture. Then, the solvent was distilled off under reduced pressure. Ethanol was added thereto, insolubles were filtered off, and the solvent was then distilled off under reduced pressure. To the resulting residue was added methanol-ethyl acetate, and then basic silica gel was added thereto. The resulting mixture was purified by basic silica gel column chromatography (methanol-ethyl acetate=1:8). The resulting solid was recrystallized from diisopropyl ether-ethyl acetate to give 5-hydroxymethyl-1-propylimidazole (33.6 g) as brown crystals.

후처리

  1. customwas returned to room temperature
  2. distillationThen, the solvent was distilled off under reduced pressure
  3. additionEthanol was added
  4. filtrationinsolubles were filtered off
  5. distillationthe solvent was then distilled off under reduced pressure
  6. additionTo the resulting residue was added methanol-ethyl acetate
  7. additionbasic silica gel was added
  8. customThe resulting mixture was purified by basic silica gel column chromatography (methanol-ethyl acetate=1:8)
  9. customThe resulting solid was recrystallized from diisopropyl ether-ethyl acetate

출처 및 근거

ORD 기록
ord-858282a6f6724ab582f25fe0768b1ba0
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07288654B2

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