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

HRID 1181867

반응식

HRID 1181867 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-220f2eafe03a453b95ad88976bb0a231
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285666B2

연결된 노트

불러오는 중…