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m-Chloroperbenzoic acid → HCID 178526231, 화합물

HRID 1506204
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HRID 1506204 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[CH:14]=[C:15]2[CH:21]=[CH:20][NH:19][C:16]2=[N:17][CH:18]=1.C(=O)([O-])O.[Na+]>C(OCC)(=O)C>[Br:12][C:13]1[CH:14]=[C:15]2[CH:21]=[CH:20][NH:19][C:16]2=[N+:17]([O-:9])[CH:18]=1
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참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 103079325-bromo-1H-pyrrolo[2,3-b]pyridine

생성물 1

HCID 178526231HCID 178526231, 화합물수율 75.4%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

m-Chloroperbenzoic acid (25 wt % water content, 322 mg, 1.40 mmol) in ethyl acetate (5 mL) was gradually added dropwise to 5-bromo-1H-pyrrolo[2,3-b]pyridine (184 mg, 0.934 mmol) in ethyl acetate (10 mL), and the reaction mixture was stirred at room temperature for 6 hours. After addition of saturated aqueous sodium hydrogen carbonate, the reaction mixture was extracted with chloroform, and the organic layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was mixed with a mixture of ethyl acetate/hexane=1/1 (v/v), and the solid was collected by filtration, washed with hexane and dried under reduced pressure to give the title compound as a light brown solid (150 mg, yield 75%).

후처리

  1. extractionthe reaction mixture was extracted with chloroform
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. additionThe residue was mixed with a mixture of ethyl acetate/hexane=1/1 (v/v)
  5. filtrationthe solid was collected by filtration
  6. washwashed with hexane
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-8aef1c7ce0404966914b68bd903ba596
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216999B2

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