Trifluoroacetic acid → HCID 178499990、化合物

HRID 642172

反応式

HRID 642172 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.C(O)(C(F)(F)F)=O.[CH3:20][O:21][C:22](=[O:52])[CH2:23][CH2:24][C:25]1[CH:30]=[CH:29][C:28]([S:31]([NH:34][C:35]2[CH:51]=[CH:50][C:38]([C:39]([NH:41][NH:42]C(OC(C)(C)C)=O)=[O:40])=[CH:37][CH:36]=2)(=[O:33])=[O:32])=[CH:27][CH:26]=1>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:42][NH:41][C:39]([C:38]1[CH:37]=[CH:36][C:35]([NH:34][S:31]([C:28]2[CH:29]=[CH:30][C:25]([CH2:24][CH2:23][C:22]([O:21][CH3:20])=[O:52])=[CH:26][CH:27]=2)(=[O:33])=[O:32])=[CH:51][CH:50]=1)=[O:40]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 886955-IodoisatinHCID 10299301Tert-butyl 2-[4-({[4-(3-methoxy-3-oxopropyl)phenyl]sulfonyl}amino)benzoyl]hydrazinecarboxylate

生成物 1

HCID 178499990HCID 178499990、化合物収率 87%

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 in the presence of 5% TFA was added tert-butyl 2-[4-({[4-(3-methoxy-3-oxopropyl)phenyl]sulfonyl}amino)benzoyl]hydrazinecarboxylate. 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. for 60 min gave 206 mg of the title compound (87%) as a yellow solid in 98.2% purity by HPLC (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. for 60 min

出典と根拠

ORDレコード
ord-29e928c5a5164c789db4468c71d6a514
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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