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

HRID 856768
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HRID 856768 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 5.0M nitric acid (370 ml) was added sodium nitrite (1.14 g), and 5-hydroxymethyl-2-mercapto-1-propylimidazole (71.0 g) was added to the mixture by portions at 0° C. The mixture was allowed to be at room temperature and the mixture was stirred for 2 hours, and water (200 ml) was added to the mixture. The mixture was neutralized with potassium carbonate at 0° C., and the solvent was distilled off under reduced pressure. Ethanol was added to the mixture, and the insolubles were filtered off, and the solvent was distilled off under reduced pressure. To the obtained residue was added methanol-ethyl acetate, and basic silica gel was added to the mixture. This mixture was purified by basic silica gel column chromatography (methanol-ethyl acetate=0.1:8), to obtain solid, which was recrystallized from diisopropyl ether-ethyl acetate, to give 5-hydroxymethyl-1-propylimidazole (33.6 g) as brown crystals.

후처리

  1. additionwas added to the mixture by portions at 0° C
  2. customto be at room temperature
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionEthanol was added to the mixture
  5. filtrationthe insolubles were filtered off
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionTo the obtained residue was added methanol-ethyl acetate, and basic silica gel
  8. additionwas added to the mixture
  9. customThis mixture was purified by basic silica gel column chromatography (methanol-ethyl acetate=0.1:8)
  10. customto obtain solid, which
  11. customwas recrystallized from diisopropyl ether-ethyl acetate

출처 및 근거

ORD 기록
ord-5c54a73fc6484e77b05d60b74edf16a0
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262185B2

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