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Hydrochloric Acid → 4-{[(2-{[5-(3,4-Dichlorophenyl)-4-hydroxy-3-thienyl]methylene}hydrazino)carbonothioyl]amino}benzoic acid

HRID 2103868
ノート
印刷プレビュー

反応式

HRID 2103868 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[S:10][CH:11]=[C:12]([CH:15]=O)[C:13]=2[OH:14])[CH:5]=[CH:6][C:7]=1[Cl:8].[NH:17]([C:19]([NH:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([OH:28])=[O:27])=[CH:24][CH:23]=1)=[S:20])[NH2:18].CN(C)C=O.Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[S:10][CH:11]=[C:12]([CH:15]=[N:18][NH:17][C:19]([NH:21][C:22]3[CH:30]=[CH:29][C:25]([C:26]([OH:28])=[O:27])=[CH:24][CH:23]=3)=[S:20])[C:13]=2[OH:14])[CH:5]=[CH:6][C:7]=1[Cl:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 27573784-(4-Carboxyphenyl)-3-thiosemicarbazideHCID 848194795-(3,4-Dichlorophenyl)-4-hydroxythiophene-3-carbaldehyde

生成物 1

HCID 723600444-{[(2-{[5-(3,4-Dichlorophenyl)-4-hydroxy-3-thienyl]methylene}hydrazino)carbonothioyl]amino}benzoic acid収率 65.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-(3,4-Dichlorophenyl)-3-hydroxy-4-formylthiophene (52 mg, 0.19 mmol) synthesized in Reference Synthetic Example 26 and 4-hydrazinocarbonothioylaminobenzoic acid (40 mg, 0.19 mmol) were stirred with dimethylformamide (1.9 mL) and concentrated hydrochloric acid (0.1 mL) at room temperature for 14 hours. Water was added to the reaction solution, and the precipitated solid was recovered by filtration and dried. The crude product was stirred with chloroform at room temperature and recovered by filtration to give the desired product as a pale yellow solid (58 mg, yield 65%).

後処理

  1. filtrationthe precipitated solid was recovered by filtration
  2. customdried
  3. filtrationrecovered by filtration

出典と根拠

ORDレコード
ord-d205f4416e0c4451a4c3f2709bae9919
出典データセット
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07576115B2

反応ノート

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