Ethyl Acetate → 7-Bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine

HRID 9184

반응식

HRID 9184 반응식
[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][CH3:12])[CH:10]=[C:6]2[CH:5]=[CH:4][CH:3]=1.F[B-](F)(F)F.[O:18]=[N+:19]=[O:20].C(OCC)(=O)C>C(#N)C>[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][CH3:12])[C:10]([N+:19]([O-:20])=[O:18])=[C:6]2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 11073463Nitronium tetrafluoroborateHCID 219845107-Bromo-2-ethylpyrazolo[1,5-a]pyridine

생성물 1

HCID 219844817-Bromo-2-ethyl-3-nitropyrazolo[1,5-a]pyridine수율 50.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

After dissolving 7-bromo-2-ethylpyrazolo[1,5-a]pyridine (1.1 g) in acetonitrile (20 mL), nitronium tetrafluoroborate (1.3 g) was added while stirring on ice, and stirring was continued for 30 minutes. The reaction mixture was added to ice water, extraction was performed with ethyl acetate and the extract was washed with water and brine. After drying over anhydrous magnesium sulfate and filtration, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (670 mg) was obtained from the n-hexane:ethyl acetate (10:1) fraction as yellow crystals.

후처리

  1. additionwas added
  2. stirringstirring
  3. washthe extract was washed with water and brine
  4. dry with materialAfter drying over anhydrous magnesium sulfate and filtration
  5. concentrationthe solvent was concentrated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9dbfc3c4f4ce448e87c72ec2f1ff0d08
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091215B2

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