反应详情

1 g of the alcohol of Example 3 was added to 220 mg of a 50% suspension of sodium hydride in oil dissolved in toluene (15 ml) and the mixture was stirred under reflux for 1 hour. 2-pyrimidinyl chloride (625 mg) in 10 ml toluene was added over 30 minutes. The mixture was stirred at reflux temperature for 16 hours. The mixture was then poured into brine and extracted with diethyl ether. The ether extract was dried over magnesium sulphate and evaporated to yield a residue which was purified on a silica gel column using 8% acetone in petrol as eluant to give 1.25 g (97%) of the desired product.

1. temperatureunder reflux for 1 hour
2. stirringThe mixture was stirred
3. temperatureat reflux temperature for 16 hours
4. extractionextracted with diethyl ether
5. extractionThe ether extract
6. dry with materialwas dried over magnesium sulphate
7. customevaporated
8. customto yield a residue which
9. customwas purified on a silica gel column