反应详情

温度

40 °C

N,N-Dimethylformamide dineopentyl acetal (2.25 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (653 mg) and 5-bromo-2-hydroxymethylthiophene (1.351 g) in dry N,N-dimethylformamide (12.5 ml) under nitrogen and then the mixture was heated at 40° C. After 2 h the temperature was increased to 80° C. After 4 h the reaction mixture was evaporated to dryness and the residue triturated with diethyl ether. The solid was collected and crystallised from acetone to give off white crystals of the title pyrimidinone (691 mg), m.p. 217°-220° C., λmax (EtOH) 243.5 nm (ε 13,810), 336 nm (ε 1,190).

1. temperatureAfter 2 h the temperature was increased to 80° C
2. customAfter 4 h the reaction mixture was evaporated to dryness
3. customthe residue triturated with diethyl ether
4. customThe solid was collected
5. customcrystallised from acetone