5-Iodoisatin → HCID 178517189、化合物

HRID 642048ノート

反応式

HRID 642048 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]1[O:14][N:15]=[C:16]2[CH:21]=[C:20]([C:22]([NH:24][NH2:25])=[O:23])[CH:19]=[CH:18][C:17]=12>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:25][NH:24][C:22]([C:20]1[CH:19]=[CH:18][C:17]2=[N:13][O:14][N:15]=[C:16]2[CH:21]=1)=[O:23]

参加物

4

反応物 2

HCID 886955-IodoisatinHCID 27354552,1,3-Benzoxadiazole-5-carbohydrazide

生成物 1

HCID 178517189HCID 178517189、化合物収率 77%

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 2,1,3-benzoxadiazole-5-carbohydrazide. 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 166 mg of the title compound (77%) as a orange solid in 99.1% purity by HPLC (Rt: 5.65, 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-48bc710da51b44988d790092b633c771
出典データセット
uspto-grants-2010_04
特許番号
US07696231B2

反応ノート

読み込み中…