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Hydrochloric Acid → 2-[N-(4-amidinophenyl)aminomethyl]benzothiazole-5-carboxylic acid-N-phenvl-N-(2-carboxyethyl)amide

HRID 50211
ノート
印刷プレビュー

反応式

HRID 50211 の反応式
[C:1]1([N:7]([CH2:30][CH2:31][C:32]([O:34]CC)=[O:33])[C:8]([C:10]2[CH:11]=[CH:12][C:13]3[S:17][C:16]([CH2:18][NH:19][C:20]4[CH:25]=[CH:24][C:23]([C:26](=[NH:28])[NH2:27])=[CH:22][CH:21]=4)=[N:15][C:14]=3[CH:29]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].Cl>C(O)C.ClCCl.C(O)C>[C:1]1([N:7]([CH2:30][CH2:31][C:32]([OH:34])=[O:33])[C:8]([C:10]2[CH:11]=[CH:12][C:13]3[S:17][C:16]([CH2:18][NH:19][C:20]4[CH:25]=[CH:24][C:23]([C:26](=[NH:27])[NH2:28])=[CH:22][CH:21]=4)=[N:15][C:14]=3[CH:29]=2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 184123862-[N-(4-amidinophenyl)aminomethyl]benzothiazole-5-carboxylic acid-N-phenyl-N-(2-ethoxycarbonylethyl)amide

生成物 1

HCID 154332162-[N-(4-amidinophenyl)aminomethyl]benzothiazole-5-carboxylic acid-N-phenvl-N-(2-carboxyethyl)amide

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒
HCID 21584144
Dichloromethane ethanol
溶媒

実験手順

0.45 g (0.84 mmol) of 2-[N-(4-amidinophenyl)aminomethyl]benzothiazole-5-carboxylic acid-N-phenyl-N-(2-ethoxycarbonylethyl)amide were dissolved in 15 mL of ethanol, mixed with 2 mL of 2N sodium hydroxide solution, and stirred for 4 hours at room temperature. Then the mixture was acidified with 3 mL of 2N hydrochloric acid and the solvent was distilled off. The crude product obtained was taken up in 5 mL dichloromethane/ethanol (2:1) and filtered to remove the insoluble sodium chloride. After the distillation of the solvent, the desired compound was obtained as a yellow foam. Yield: 0.26 g (67% of theory), C25H23N5O3S (473.55); Rf value: 0.47 (silica gel; methanol/5% aqueous sodium chloride=6:4); mass spectrum: (M+H)+=474.

後処理

  1. distillationthe solvent was distilled off
  2. customThe crude product obtained
  3. filtrationfiltered
  4. customto remove the insoluble sodium chloride
  5. distillationAfter the distillation of the solvent

出典と根拠

ORDレコード
ord-7ed778732f9a445f90543cdba1ed91a2
出典データセット
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06710055B2

反応ノート

読み込み中…

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