反应详情

2-(2-Thienylmethylthio)ethylamine hydrochloride (2 g) in ethanol (25 ml) was added to a solution of sodium ethoxide (prepared from 0.218 g sodium) in ethanol and the mixture was stirred for 0.5 hour. 2-Nitroamino-5-(3-pyridylmethyl)-4-pyrimidone (2.34 g) was added and the mixture was boiled under reflux for 40 hours and evaporated to dryness. Pyridine (50 ml) was added to the residue and the mixture was boiled under reflux for 24 hours and evaporated. The residue was crystallised from ethanol/ethyl acetate and further purified by elution from a column of silica gel with ethyl acetate/methanol (5:1) and recrystallisation from 2-propanol to give 2-[2-(2-thienylmethylthio)ethylamino]-5-(3-pyridylmethyl)-4-pyrimidone m.p. 145°-148°.

1. temperatureunder reflux for 40 hours
2. customevaporated to dryness
3. additionPyridine (50 ml) was added to the residue
4. temperatureunder reflux for 24 hours
5. customevaporated
6. customThe residue was crystallised from ethanol/ethyl acetate
7. customfurther purified by elution from a column of silica gel with ethyl acetate/methanol (5:1) and recrystallisation from 2-propanol