Pyridine → HCID 13176887, Verbindung

HRID 371426

Reaktionsgleichung

Reaktionsgleichung von HRID 371426
N1C=CC=CC=1.[CH2:7]([O:14][C:15]([NH:17][CH2:18][C:19]1[CH:27]=[CH:26][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=1)=[O:16])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C1CCC(N=C=NC2CCCCC2)CC1.CS(O[C:48]1[CH:57]=[CH:56][C:55]2[C:50](=[CH:51][CH:52]=[C:53]([C:58](=[NH:60])[NH2:59])[CH:54]=2)[CH:49]=1)(=O)=O>C(OCC)C>[CH2:7]([O:14][C:15]([NH:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([C:23]([O:25][C:48]2[CH:57]=[CH:56][C:55]3[C:50](=[CH:51][CH:52]=[C:53]([C:58](=[NH:59])[NH2:60])[CH:54]=3)[CH:49]=2)=[O:24])=[CH:26][CH:27]=1)=[O:16])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1

Komponenten

6

Edukt 4

HCID 1049PyridineHCID 10868DicyclohexylcarbodiimideHCID 14799974-((((Benzyloxy)carbonyl)amino)methyl)benzoic acidHCID 13050560HCID 13050560, Verbindung

Produkt 1

HCID 13176887HCID 13176887, VerbindungAusbeute 46,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

To 50 ml of dried pyridine, were added 5.1 g of 4-benzyloxycarbonylaminomethylbenzoic acid and 4.4 g of DCC. The mixture was stirred under cooling in ice for 30 minutes, admixed with 5.0 g of 6-amidino-2-naphthol methanesulfonate and stirred for one hour under cooling in ice, then overnight at room temperature. The reaction mixture was filtered* and the filtrate was mixed with ethyl ether. The precipitate which was formed was collected by filtration and recrystallized from a DMF-ethanol mixture to obtain 3.8 g of a white powder of a white powder of 6-amidino-2-naphthyl 4-benzyloxycarbonylaminomethylbenzoate methanesulfonate.

Aufarbeitung

  1. temperatureunder cooling in ice for 30 minutes
  2. stirringstirred for one hour
  3. temperatureunder cooling in ice
  4. customovernight
  5. customat room temperature
  6. customThe precipitate which was formed
  7. filtrationwas collected by filtration
  8. customrecrystallized from a DMF-ethanol mixture

Quellen und Nachweise

ORD-Eintrag
ord-9e5fc2c2395f4db097b15096d444a484
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04532255

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