反应详情

Sodium metal (1.01 g, 44 mmol) was added to ethanol (100 ml) and stirred until all the metal had dissolved. Ethylacetoacetate (15.6 g, 111 mmol) was added and the reaction mixture was stirred under a nitrogen atmosphere for 10 minutes. 3,5-dichlorobenzyl chloride (7.24 g, 40 mmol) was added and the reaction mixture was stirred at room temperature for 3 days. The reaction mixture was filtered and the solution was concentrated under reduced pressure. The orange oil was purified by flash chromatography on silica gel eluting with pentane followed by pentane:ethyl acetate (30:1, by volume) to afford the title compound as a colourless oil (6.4 g).

1. dissolutionhad dissolved
2. stirringthe reaction mixture was stirred under a nitrogen atmosphere for 10 minutes
3. stirringthe reaction mixture was stirred at room temperature for 3 days
4. filtrationThe reaction mixture was filtered
5. concentrationthe solution was concentrated under reduced pressure
6. customThe orange oil was purified by flash chromatography on silica gel eluting with pentane