Hydrochloric Acid → HCID 178485721, Verbindung

HRID 482264Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 482264
[ClH:1].[C:2]([C:4]([C:17](=[O:30])[N:18]([CH3:29])[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:28])([F:27])[F:26])[CH:20]=1)=[CH:5][NH:6][C:7](=[NH:16])[N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15])#[N:3]>CCOCC.C(O)C>[ClH:1].[C:2]([C:4]([C:17](=[O:30])[N:18]([CH3:29])[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([C:25]([F:26])([F:27])[F:28])[CH:20]=1)=[CH:5][NH:6][C:7](=[NH:16])[N:8]1[CH2:12][C:11]([CH3:14])([CH3:13])[NH:10][C:9]1=[O:15])#[N:3]

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 178485720HCID 178485720, Verbindung2×

Produkt 1

HCID 178485721HCID 178485721, VerbindungAusbeute 90,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

3.1 ml of a 6.6 molar solution of HCl in ether were added dropwise to a suspension of 8.17 g (20 mmol) of 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]-ethene (compound IV) in 48 ml of ethanol at room temperature, and the mixture was stirred at 1°-3° C. for 1 hour. The solid was then filtered off with suction, washed with ether and dried at room temperature in vacuo (4-6 mbar) for 20 hours. 8.34 g (=90.7% yield) of pure 1-cyano-1-[N-methyl-N-(3-trifluoromethylphenyl)carbamoyl]-2-[imino-(4,4-dimethyl-2-oxo-1-imidazolidinyl)methylamino]ethene hydrochloride were obtained, melting point 180°-181° C. (=transition point; substance resolidifies); C18H20ClF3N6O2 (444.86)

Aufarbeitung

  1. filtrationThe solid was then filtered off with suction
  2. washwashed with ether
  3. customdried at room temperature in vacuo (4-6 mbar) for 20 hours

Quellen und Nachweise

ORD-Eintrag
ord-6a1e8720a3834f7c8cdd69406e8f0570
Quelldatensatz
uspto-grants-1998_08
Patentnummer
US05795899

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