Reaktion #2253877

Reaktionsgleichung

2-(5-methyl-4-imidazolylmethylthio)ethylamine

2-nitroamino-5-(5-dimethylaminomethyl-2-thienylmethyl)-4-pyrimidone

→

2-[2-(5-methyl-4-imidazolyl-methylthio)ethylamino]-5-(5-dimethylaminomethyl-2-thienylmethyl)-4-pyrimidone

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 48 hrs
3. 3
   SonstigeThe ethanol was evaporated at reduced pressure

Vorschrift

A mixture of 2-(5-methyl-4-imidazolylmethylthio)ethylamine (1.37 g) and 2-nitroamino-5-(5-dimethylaminomethyl-2-thienylmethyl)-4-pyrimidone (2.32 g) in ethanol was heated under reflux for 48 hrs. The ethanol was evaporated at reduced pressure yielding 2-[2-(5-methyl-4-imidazolyl-methylthio)ethylamino]-5-(5-dimethylaminomethyl-2-thienylmethyl)-4-pyrimidone as a glassy residue which was washed with hot water by decantation. The residue was dissolved in isopropanol and a solution of ethanolic hydrochloric acid (3 ml) was added. Excess of solvent was removed at reduced pressure and trihydrochloride crystallized as a light buff solid (3.11 g). The solid was recrystallized from methanol-ethanol (2.36 g) 185.5°-188.5° C.

Quelle