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5-Chlorooxindole → N-isobutyryl-5-chloro-2-oxindole-1-carboxamide

HRID 637361
ノート
印刷プレビュー

反応式

HRID 637361 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[CH2:5]2.[C:12]([N:17]=[C:18]=[O:19])(=[O:16])[CH:13]([CH3:15])[CH3:14]>C1(C)C=CC=CC=1>[C:12]([NH:17][C:18]([N:7]1[C:8]2[C:4](=[CH:3][C:2]([Cl:1])=[CH:10][CH:9]=2)[CH2:5][C:6]1=[O:11])=[O:19])(=[O:16])[CH:13]([CH3:15])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1528015-ChlorooxindoleHCID 127486372-Methylpropanecarbonyl isocyanate

生成物 1

HCID 13647652N-isobutyryl-5-chloro-2-oxindole-1-carboxamide収率 23%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred slurry of 8.38 g (0.05 mole) of 5-chloro-2-oxindole in 250 ml of toluene was added 6.79 g (0.06 mole) of isobutyryl isocyanate, and the reaction mixture was heated under reflux for 5.5 hours. The reaction mixture was cooled to room temperature, a small amount of insoluble material was removed by filtration, and then the solvent was removed by evaporation in vacuo. The residue was recrystallized from acetonitrile (with the aid of decolorizing carbon), followed by recrystallization from ethanol, to give 3.23 g of the title compound as pink crystals, m.p. 139°-141° C.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 5.5 hours
  3. customa small amount of insoluble material was removed by filtration
  4. customthe solvent was removed by evaporation in vacuo
  5. customThe residue was recrystallized from acetonitrile (with the aid of decolorizing carbon),
  6. customfollowed by recrystallization from ethanol

出典と根拠

ORDレコード
ord-4141470d1ce646a6b2d9c4e9de47d987
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04556672

反応ノート

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