Water → 1-Allyl-1H-pyrazole-5-carbaldehyde

HRID 31544

반응식

HRID 31544 반응식
[NH:1]1[CH:5]=[CH:4][C:3]([CH:6]=[O:7])=[N:2]1.C(=O)([O-])[O-].[K+].[K+].[CH2:14](Br)[CH:15]=[CH2:16].O>CN(C=O)C>[CH2:16]([N:2]1[C:3]([CH:6]=[O:7])=[CH:4][CH:5]=[N:1]1)[CH:15]=[CH2:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 122183831H-Pyrazole-3-carbaldehyde

생성물 1

HCID 235104011-Allyl-1H-pyrazole-5-carbaldehyde수율 10.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Pyrazole-3-carbaldehyde (3.00 g, 31.2 mmol) was dissolved in DMF (20 ml), and thereto were added potassium carbonate (6.47 g, 46.8 mmol) and allyl bromide (3.50 g, 32.8 mmol) with stirring. The mixture was stirred at room temperature for 6 hours, and thereto was added water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated saline, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the resulting residue was purified by silica gel column chromatography to give the title compound (429 mg, 10%).

후처리

  1. stirringThe mixture was stirred at room temperature for 6 hours
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customthe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-fbfff4f61fb142d68d6b767e74c32fa3
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425642B2

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