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

HRID 1864992

반응식

HRID 1864992 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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 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.

후처리

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

출처 및 근거

ORD 기록
ord-5209caacfde747999a6936f9d9fb3657
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625925B2

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