反应详情

A mixture of 5-chloropyrimidin-2-one (522 mg) and 2-(2-bromopropionyl)thiophene (965 mg) in triethylamine (0.84 ml) and ethanol (25 ml) was stirred at room temperature. After 3 h. the mixture was heated to 50° C. After a further 1 h. the solvent was removed and the residue dissolved in ethyl acetate (50 ml) which was washed with water (3×25 ml) and brine, dried (MgSO4) and evaporated to a yellow oil. The oil was triturated with diethyl ether and the resulting solid was crystallised twice from ethyl acetate to give the title pyrimidinone (320 mg), m.p. 128°-129° C., λmax (EtOH) 226 nm (ε 11,340), 263 nm (ε10,050), 290 nm (ε 8,950).

1. temperatureAfter 3 h. the mixture was heated to 50° C
2. customAfter a further 1 h. the solvent was removed
3. dissolutionthe residue dissolved in ethyl acetate (50 ml) which
4. washwas washed with water (3×25 ml) and brine
5. dry with materialdried (MgSO4)
6. customevaporated to a yellow oil
7. customThe oil was triturated with diethyl ether
8. customthe resulting solid was crystallised twice from ethyl acetate