反应详情

A 60% mineral oil suspension of sodium hydride (12.7 g, 0.31 mole) in dimethylformamide under nitrogen, is treated with cyano-2,2-dimethylcyclopentanone over a 50 minute period at ice-bath temperatures, then with a solution of 4-chloro-benzyl chloride (50.2 g, 0.31 mole) over a 30 minute period, stirred for 5 hours and quenched with water. The resultant mixture is extracted with ethyl acetate. The extracts are combined, washed with water and concentrated in vacuo to afford a solid residue. The residue is titurated with hexane to afford the title product as white crystals, 59.3 g (72.6% yield), mp 101°-103° C., identified by gas chromatography.

1. customquenched with water
2. extractionThe resultant mixture is extracted with ethyl acetate
3. washwashed with water
4. concentrationconcentrated in vacuo
5. customto afford a solid residue