5-Bromoisatin → HCID 178498288、化合物

HRID 642120

反応式

HRID 642120 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=O.[NH:13]([C:15](=[O:28])[CH2:16][O:17][C:18]1[CH:27]=[CH:26][C:21]([C:22]([O:24][CH3:25])=[O:23])=[CH:20][CH:19]=1)[NH2:14]>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6](=[O:11])[C:5]2=[N:14][NH:13][C:15](=[O:28])[CH2:16][O:17][C:18]1[CH:27]=[CH:26][C:21]([C:22]([O:24][CH3:25])=[O:23])=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 68895-BromoisatinHCID 2759745Methyl 4-((aminocarbamoyl)methoxy)benzoate

生成物 1

HCID 178498288HCID 178498288、化合物収率 80%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

Following the general method as outlined in Example 1, into a suspension of 5-bromo-1H-indole-2,3-dione in acetic acid was added methyl 4(2-hydrazino-2-oxoethoxy)benzoate. After stirring at 100° C., the reaction mixture was cooled to rt and a yellow solid precipitated out. Filtration on a fritté, washing with AcOH, water and drying under vacuo at 60° C. overnight gave 86 mg of the title compound (80%) as a orange powder in 94% purity by HPLC (Rt: 4.17, gradient of 8 min, MaxPlot detection between 230 and 400 nm).

後処理

  1. temperaturethe reaction mixture was cooled to rt
  2. customa yellow solid precipitated out
  3. filtrationFiltration on a fritté
  4. washwashing with AcOH, water
  5. customdrying under vacuo at 60° C. overnight

出典と根拠

ORDレコード
ord-ba222646a9754250878e4cc9a82abea4
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

関連ノート

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