1-Methylthio-1-methylamino-2-nitroethylene → 1-[3-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethylene

HRID 34781

Reaktionsgleichung

Reaktionsgleichung von HRID 34781
[F:1][C:2]([F:20])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][CH2:16][NH2:17])[N:8]=1.[CH3:21][NH:22][C:23](SC)=[CH:24][N+:25]([O-:27])=[O:26]>C(#N)C>[F:20][C:2]([F:1])([F:19])[CH2:3][N:4]=[C:5]([NH2:18])[NH:6][C:7]1[CH:12]=[CH:11][N:10]=[C:9]([S:13][CH2:14][CH2:15][CH2:16][NH:17][C:23]([NH:22][CH3:21])=[CH:24][N+:25]([O-:27])=[O:26])[N:8]=1

Komponenten

4

Edukt 2

HCID 1235491-Methylthio-1-methylamino-2-nitroethyleneHCID 212987114-[2-(2,2,2-Trifluoroethyl)guanidino]-2-(3-aminopropylthio)pyrimidine

Produkt 1

HCID 704179461-[3-(4-[2-(2,2,2-Trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethyleneAusbeute 26,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of 4-[2-(2,2,2-trifluoroethyl)guanidino]-2-(3-aminopropylthio)pyrimidine (0.31 g.) in acetonitrile (5 ml.) was treated with 1-methylamino-1-methylthio-2-nitroethylene (0.15 g.) and the mixture heated under reflux for 18 hours. The hot solution was filtered and cooled and the solid which crystallised was collected and recrystallised from ethanol to give 1-[3-(4-[2-(2,2,2-trifluoroethyl)guanidino]pyrimid-2-ylthio)propylamino]-1-methylamino-2-nitroethylene (0.11 g.), m.p. 189°-191°.

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 18 hours
  3. filtrationThe hot solution was filtered
  4. temperaturecooled
  5. customthe solid which crystallised
  6. customwas collected
  7. customrecrystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-55894688c5ab4642bc637db5c9cec5c3
Quelldatensatz
uspto-grants-1988_08
Patentnummer
US04762932

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