Reaktion #1991265

Reaktionsgleichung

2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine

2-nitroamino-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone

→

2-[2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamino]-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone

Ausbeute 40.7%

Lösungsmittel

pyridine

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux for 5 hours
3. 3
   Sonstigeevaporated to dryness in vacuo
4. 4
   SonstigeThe residue was purified by chromatography on silica gel
5. 5
   Wascheneluted with 20% methanol/chloroform
6. 6
   Sonstigefollowed by recrystallisation from acetonitrile/water 1:1

Vorschrift

A mixture of 2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamine (1 g) and 2-nitroamino-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone (1.11 g) in pyridine (3 ml) was heated under reflux for 5 hours and evaporated to dryness in vacuo. The residue was purified by chromatography on silica gel eluted with 20% methanol/chloroform followed by recrystallisation from acetonitrile/water 1:1 to give 2-[2-(4-dimethylaminomethyl-2-pyridylmethylthio)ethylamino]-5-(5,6-dimethyl-3-pyridylmethyl)-4-pyrimidone (0.72 g) m.p. 72°-78°.

Quelle