m-Chloroperbenzoic acid → HCID 178422841, 화합물

HRID 872042노트

반응식

HRID 872042 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][C:13]1[N:18]=[C:17]2[NH:19][CH:20]=[CH:21][C:16]2=[CH:15][CH:14]=1>C(OCC)(=O)C.C(=O)([O-])[O-].[K+].[K+]>[CH3:12][C:13]1[N+:18]([O-:9])=[C:17]2[NH:19][CH:20]=[CH:21][C:16]2=[CH:15][CH:14]=1

참가 물질

5

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 114577166-Methyl-1H-pyrrolo[2,3-b]pyridine

생성물 1

HCID 178422841HCID 178422841, 화합물수율 90%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 11430Potassium Carbonate용매

실험 절차

65% m-Chloroperbenzoic acid (1374 mg) was added to a solution of 6-methyl-1H-pyrrolo[2,3-b]pyridine (570 mg) in ethyl acetate (20 ml) under ice-cooling and the mixture was stirred at room temperature for 20 minutes. After concentration of the reaction mixture in vacuo, the resulted residue was diluted with 2% aqueous solution of potassium carbonate and extracted with chloroform. The organic layer was dried over magnesium sulfate and concentrated in vacuo. The resulted residue was purified with a NH-silica gel column chromatography (eluting solvent: chloroform/methanol=30/1 to 9/1) to give 6-methyl-1H-pyrrolo[2,3-b]pyridin-7-oxide (575 mg) as a colorless powder.

후처리

  1. temperaturecooling
  2. extractionextracted with chloroform
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe resulted residue was purified with a NH-silica gel column chromatography (eluting solvent: chloroform/methanol=30/1 to 9/1)

출처 및 근거

ORD 기록
ord-78e521754ff64888ac0b1ac6680e5286
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08975252B2

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