反应详情

A mixture of methyl cyanoacetate (1.3 ml, 15×10−3 mol), of solketal (1.25 ml, 10×10−3 mol) and of DMAP (2.7 mg, 0.03 equiv.) is heated at reflux with stirring for 30 hours in a reactor rendered inert with nitrogen. After cooling, the solvent is evaporated under vacuum and the brown oil obtained is chromatographed on a silica column (gradient of eluents: heptane/EtOAc from 90:10 to 80:20). 423 mg (yield: 23%) of the pure fractions of (2,2-dimethyl-1,3-dioxolan-4-yl)methyl cyanoacetate are thus obtained in the form of a yellow oil used as is in the following stage.

1. temperatureat reflux
2. temperatureAfter cooling
3. customthe solvent is evaporated under vacuum
4. customthe brown oil obtained
5. customis chromatographed on a silica column (gradient of eluents: heptane/EtOAc from 90:10 to 80:20)