5-Iodoisatin → HCID 178442529、化合物

HRID 642076ノート

反応式

HRID 642076 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.[CH2:13]([C:20]1[CH:38]=[CH:37][C:23]([C:24]([NH:26][C:27]2[CH:32]=[CH:31][C:30]([C:33]([NH:35][NH2:36])=[O:34])=[CH:29][CH:28]=2)=[O:25])=[CH:22][CH:21]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>C(O)(=O)C>[CH2:13]([C:20]1[CH:38]=[CH:37][C:23]([C:24]([NH:26][C:27]2[CH:28]=[CH:29][C:30]([C:33]([NH:35][N:36]=[C:5]3[C:4]4[C:8](=[CH:9][CH:10]=[C:2]([I:1])[CH:3]=4)[NH:7][C:6]3=[O:11])=[O:34])=[CH:31][CH:32]=2)=[O:25])=[CH:22][CH:21]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]

参加物

4

反応物 2

HCID 886955-IodoisatinHCID 101327784-heptyl-N-[4-(hydrazinocarbonyl)phenyl]benzamide

生成物 1

HCID 178442529HCID 178442529、化合物収率 91%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

Into a suspension of 5-iodo-1H-indole-2,3-dione in acetic acid was added 4-heptyl-N-[4-(hydrazinocarbonyl)phenyl]-benzamide. 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 111 mg of the title compound (91%) as a yellow powder in 93.1% purity by HPLC (Rt: 6.3, gradient of 8 min, MaxPlot detection between 230 and 400 nm).

後処理

  1. temperaturewas 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-35fe224cdf2345598a2793d8fd4a148a
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

反応ノート

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