Ethyl Acetate → 7-(2,4-Dichlorophenyl)-2-ethyl-3-nitropyrazolo[1,5-a]pyridine

HRID 9183

反応式

HRID 9183 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]2[N:15]=[C:16]([CH2:18][CH3:19])[CH:17]=[C:13]2[CH:12]=[CH:11][CH:10]=1.F[B-](F)(F)F.[O:25]=[N+:26]=[O:27].C(OCC)(=O)C>C(#N)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]2[N:15]=[C:16]([CH2:18][CH3:19])[C:17]([N+:26]([O-:27])=[O:25])=[C:13]2[CH:12]=[CH:11][CH:10]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 11073463Nitronium tetrafluoroborateHCID 219846357-(2,4-Dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine

生成物 1

HCID 219846667-(2,4-Dichlorophenyl)-2-ethyl-3-nitropyrazolo[1,5-a]pyridine収率 35.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

After dissolving 7-(2,4-dichlorophenyl)-2-ethylpyrazolo[1,5-a]pyridine (280 mg) in acetonitrile (20 mL), nitronium tetrafluoroborate (255 mg) was added 4 times at 30 minute intervals while stirring on ice. 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 (115 mg) was obtained from the n-hexane:ethyl acetate (20:1) fraction as yellow crystals.

後処理

  1. additionwas added 4 times at 30 minute intervals
  2. washthe extract was washed with water and brine
  3. dry with materialAfter drying over anhydrous magnesium sulfate and filtration
  4. concentrationthe solvent was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-b0d69462f11d46589ba57d6318c7fae0
出典データセット
uspto-grants-2006_08
特許番号
US07091215B2

関連ノート

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