反应详情

温度

90 °C

N,N-Dimethylformamide dineopentyl acetal (1.8 ml) was added to a stirred suspension of 5-chloropyrimidin-2-one (522 mg) and 4-pyridylcarbinol (611 mg) in dry N,N-dimethylformamide (10 ml) under nitrogen and the the mixture was then heated at 90° C. After 41/2 h the reaction mixture was evaporated to a brown solid which was subjected to column chromatography on silica developing and eluting with chloroform-ethanol, 14:1. This gave a yellow crystalline solid which was subjected to p.l.c. on silica developing with chloroform-ethanol, 9:1 (three runs). The major band was eluted with chloroform-ethanol, 1:1, to give a pale yellow foam which was crystallised from acetone to give off white crystals of the title pyrimidinone (210 mg), m.p. 205°-206° C., λmax (EtOH) 246 nm (ε 7.050), 332.5 nm (ε 950).

1. customAfter 41/2 h the reaction mixture was evaporated to a brown solid which
2. washeluting with chloroform-ethanol, 14:1
3. customThis gave a yellow crystalline solid which
4. washThe major band was eluted with chloroform-ethanol, 1:1
5. customto give a pale yellow foam which
6. customwas crystallised from acetone