5-Iodoisatin → HCID 178521411、化合物

HRID 642082

反応式

HRID 642082 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.[NH:13]([C:15](=[O:27])[CH2:16][O:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([OH:24])=[O:23])=[CH:20][CH:19]=1)[NH2:14]>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:14][NH:13][C:15](=[O:27])[CH2:16][O:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([OH:24])=[O:23])=[CH:20][CH:19]=1

参加物

4

反応物 2

HCID 886955-IodoisatinHCID 98558384-(2-Hydrazino-2-oxoethoxy)benzoic acid

生成物 1

HCID 178521411HCID 178521411、化合物収率 7%

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-(2-hydrazino-2-oxoethoxy)benzoic acid. 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 6 mg of the title compound (7%) as a yellow solid in 97.8% purity by HPLC (Rt: 3.63, 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-4cc616046cfb4ab3a5b2e3b600b04a85
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

関連ノート

読み込み中…