反应详情

A mixture of 33.3 g of 4-(1E-pentenyl)cyclohexanone (prepared in accordance with EP-A-168683), 42 ml of ethyl cyanoacetate, 300 ml of toluene and 2.9 g of piperidinium acetate is boiled for 1.5 hours on a water separator. After cooling the reaction mixture is washed with three 50 ml portions of water, dried over sodium sulphate and concentrated. Chromatographic purification of the residue on 750 g of silica gel with hexane/ethyl acetate (vol. 19:1) gives ethyl cyano-[4-(1E-pentenyl)cyclohexylidene]-acetate.

1. temperatureAfter cooling the reaction mixture
2. washis washed with three 50 ml portions of water
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated
5. customChromatographic purification of the residue on 750 g of silica gel with hexane/ethyl acetate (vol. 19:1)