Methanol → 1-(6-Chloro-3-pyridylmethyl)-3-methyl2-nitroguanidine

HRID 1069385Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1069385
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][N:9]2CN(CCC)[CH2:12][N:11](C)[C:10]2=[N:19][N+:20]([O-:22])=[O:21])=[CH:4][N:3]=1.C(=O)([O-])O.[Na+].CO>O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10]([NH:11][CH3:12])=[N:19][N+:20]([O-:22])=[O:21])=[CH:4][N:3]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 516892Sodium BicarbonateHCID 541470021-(2-Chloropyrid-5-ylmethyl)-2-nitroimino-3-methyl-5-n-propyl-1,3,5-triazacyclohexane

Produkt 1

HCID 1362181961-(6-Chloro-3-pyridylmethyl)-3-methyl2-nitroguanidine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture of 1.5 g of 1-(2-chloropyrid-5-ylmethyl)-2-nitroimino-3-methyl-5-n-propyl-1,3,5-triazacyclohexane, 0.5 g of solid sodium hydrogen carbonate, 20 ml of methanol and 10 ml of water is stirred for 24 hours at 50° C. The reaction mixture is concentrated by evaporation and the residue purified on silica gel with dichloromethane/methanol 95:5 as the eluant. This yields the title compound with a melting point of 149-151° C. (compound 2.2).

Aufarbeitung

  1. concentrationThe reaction mixture is concentrated by evaporation
  2. customthe residue purified on silica gel with dichloromethane/methanol 95:5 as the eluant

Quellen und Nachweise

ORD-Eintrag
ord-4fa5d045bc534b3fbc12080bb9db4e62
Quelldatensatz
uspto-grants-2001_06
Patentnummer
US06252072B1

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