5-Iodoisatin → HCID 178517197、化合物

HRID 642041

反応式

HRID 642041 の反応式
[I: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.[N+:13]([C:16]1[CH:17]=[C:18]([CH:23]=[CH:24][CH:25]=1)[C:19]([NH:21][NH2:22])=[O:20])([O-:15])=[O:14]>C(O)(=O)C>[I: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:22][NH:21][C:19](=[O:20])[C:18]1[CH:23]=[CH:24][CH:25]=[C:16]([N+:13]([O-:15])=[O:14])[CH:17]=1

参加物

4

反応物 2

HCID 886955-IodoisatinHCID 32914983-Nitrobenzohydrazide

生成物 1

HCID 178517197HCID 178517197、化合物収率 81%

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-iodo-1H-indole-2,3-dione in acetic acid was added 3-nitrobenzohydrazide. 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 176 mg of the title compound (81%) as a orange solid in 98.4% purity by HPLC (Rt: 5.61, gradient of 10 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-e441c282224445459a4f717d6b7a9597
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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