反应详情

A mixture of 25.0 g of cyclodecanone, 60.7 g of diethyl aminomethylenemalonate, 1.54 g of p-toluenesulfonic acid monohydrate in 500 ml xylene is refluxed 2 weeks under argon, collecting the distillate in a Dean-Stark trap. The solution is then decanted and solvent is removed. The residual oil is triturated twice with hexane and the combined hexane extract is concentrated to yield an oil which is flash chromatographed on 600 g of silica gel using 99:1 methylene chloride ethyl acetate as eluent. A forerun containing cyclodecanone is discarded and the fractions containing the product are combined and concentrated to dryness to give diethyl N-(1-cyclodecenyl)-aminomethylenemalonate as an oil.

1. temperatureis refluxed 2 weeks under argon
2. distillationcollecting the distillate in a Dean-Stark trap
3. customThe solution is then decanted
4. customsolvent is removed
5. customThe residual oil is triturated twice with hexane
6. extractionthe combined hexane extract
7. concentrationis concentrated
8. customto yield an oil which
9. customchromatographed on 600 g of silica gel using 99:1 methylene chloride ethyl acetate as eluent
10. additionA forerun containing cyclodecanone
11. additionthe fractions containing the product
12. concentrationconcentrated to dryness