m-Chloroperbenzoic acid → HCID 178422841、化合物

HRID 872042ノート

反応式

HRID 872042 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 178422841HCID 178422841、化合物収率 90%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 11430Potassium Carbonate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-78e521754ff64888ac0b1ac6680e5286
出典データセット
uspto-grants-2015_03
特許番号
US08975252B2

反応ノート

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