反应详情

A mixture of n-butanol (5 ml) and sodium hydride (60% in oil, 10 mmol) is stirred until the formation of H2 gas ceases. A mixture of 1C (0.7 g, 2,2 mmol) and dimethoxyethane (15 ml) is added to the resulting reaction mixture. Subsequently, the reaction mixture is heated under reflux with stirring for 24 hours. A mixture of water and ethyl acetate (1:1 v/v; 100 ml) is then slowly added at room temperature. The organic phase is separated, concentrated and the residue is purified by column chromatography (petrol ether: ethyl acetate, 95:5 v/v) yielding the pure product as a yellow oil, 0.2 g, (24.4%).

1. additionis added to the resulting reaction mixture
2. temperatureSubsequently, the reaction mixture is heated
3. temperatureunder reflux
4. stirringwith stirring for 24 hours
5. additionis then slowly added at room temperature
6. customThe organic phase is separated
7. concentrationconcentrated
8. customthe residue is purified by column chromatography (petrol ether: ethyl acetate, 95:5 v/v)