Water → 7-Bromo-2-ethyl-4-methoxy-3-nitropyrazolo[1,5-a]pyridine

HRID 9190

反応式

HRID 9190 の反応式
F[B-](F)(F)F.[O:6]=[N+:7]=[O:8].[Br:9][C:10]1[N:15]2[N:16]=[C:17]([CH2:19][CH3:20])[CH:18]=[C:14]2[C:13]([O:21][CH3:22])=[CH:12][CH:11]=1.O>C(#N)C>[Br:9][C:10]1[N:15]2[N:16]=[C:17]([CH2:19][CH3:20])[C:18]([N+:7]([O-:8])=[O:6])=[C:14]2[C:13]([O:21][CH3:22])=[CH:12][CH:11]=1

参加物

5

反応物 3

HCID 962WaterHCID 11073463Nitronium tetrafluoroborateHCID 219845677-Bromo-2-ethyl-4-methoxypyrazolo[1,5-a]pyridine

生成物 1

HCID 219845347-Bromo-2-ethyl-4-methoxy-3-nitropyrazolo[1,5-a]pyridine収率 47.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

After adding nitronium tetrafluoroborate (176 mg) to a solution of 7-bromo-2-ethyl-4-methoxypyrazolo[1,5-a]pyridine (282 mg) in acetonitrile (20 mL) at 0° C., the mixture was stirred for 20 minutes. Upon completion of the reaction, water was added, extraction was performed with ethyl acetate, the extract was washed with saturated aqueous sodium hydrogencarbonate and brine and dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (20 g), and the title compound (159 mg) was obtained from the n-hexane:ethyl acetate (3:1) fraction as yellow crystals.

後処理

  1. additionwas added
  2. extractionextraction
  3. washthe extract was washed with saturated aqueous sodium hydrogencarbonate and brine
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-6d8efc54b4a14188bbf41ce10a29232f
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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