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Hydrogen Peroxide → 1-Methyl-2-[(4-amidinophenyl)sulfonylmethyl]benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)amide Hydrochloride

HRID 2288471
ノート
印刷プレビュー

反応式

HRID 2288471 の反応式
[ClH:1].C(N(CCC(OCC)=O)C(C1C=CC2N(C)C(CSC3C=CC(C(=N)N)=CC=3)=NC=2C=1)=[O:7])CC.OO.Cl.[CH2:39]([N:42]([CH2:67][CH2:68][C:69]([O:71][CH2:72][CH3:73])=[O:70])[C:43]([C:45]1[CH:66]=[CH:65][C:48]2[N:49]([CH3:64])[C:50]([CH2:52][S:53]([C:55]3[CH:60]=[CH:59][C:58]([C:61](=[NH:63])[NH2:62])=[CH:57][CH:56]=3)=[O:54])=[N:51][C:47]=2[CH:46]=1)=[O:44])[CH2:40][CH3:41].C(OCC)(=O)C.C(O)C>C(O)=O>[ClH:1].[CH2:39]([N:42]([CH2:67][CH2:68][C:69]([O:71][CH2:72][CH3:73])=[O:70])[C:43]([C:45]1[CH:66]=[CH:65][C:48]2[N:49]([CH3:64])[C:50]([CH2:52][S:53]([C:55]3[CH:60]=[CH:59][C:58]([C:61](=[NH:62])[NH2:63])=[CH:57][CH:56]=3)(=[O:7])=[O:54])=[N:51][C:47]=2[CH:46]=1)=[O:44])[CH2:40][CH3:41]
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 784Hydrogen PeroxideHCID 184124111-methyl-2-[(4-amidinophenyl)thiomethyl]benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)amide hydrochlorideHCID 184126971-methyl-2-[(4-amidinophenyl)sulfinylmethyl]benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)amide hydrochlorideHCID 21584252Ethanol ethylacetate

生成物 1

HCID 18412681
1-Methyl-2-[(4-amidinophenyl)sulfonylmethyl]benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)amide Hydrochloride
収率 95%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

A solution of 0.40 g (0.70 mMol) of 1-methyl-2-[(4-amidinophenyl)thiomethyl]-benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)-amide-hydrochloride in 10 ml of formic acid was mixed with 2 ml of 30% hydrogen peroxide solution and the mixture was stirred for 16 hours at room temperature. Then the solvent was distilled off in vacuo, whereupon the desired compound was obtained as a beige solid (contaminated with some 1-methyl-2-[(4-amidinophenyl)sulfinylmethyl]-benzimidazol-5-yl-carboxylic acid-N-(n-propyl)-N-(2-ethoxycarbonylethyl)-amide-hydrochloride). Yield: 95% of theory, C25H31N6O5S (513.62) Rf value: 0.50 (silica gel; ethyl acetate/ethanol/1N hydrochloric acid =50:45:5) EKA mass spectrum: (M+H)+ =514

後処理

  1. distillationThen the solvent was distilled off in vacuo, whereupon the desired compound
  2. customwas obtained as a beige solid (

出典と根拠

ORDレコード
ord-0fc27946e8f343e0ab8ed4930fb8f3bc
出典データセット
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06087380

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート