反应详情

33.9 mL (0.223 mol) of diethyl malonate were added, under a nitrogen atmosphere and at room temperature, to a solution of sodium ethoxide (prepared in situ by dissolving 2.6 g (0.0151 mol) of Na in 80 mL of absolute EtOH). After 30 min, 14.5 g (0.0677 mol) of 2-methylphenethyl alcohol methanesulphonate dissolved in 40 mL of abs. EtOH were added dropwise and the resulting solution was heated to reflux for 3 h. EtOH was removed in vacuo, the residue was taken up in water and extracted with Et2O. The organic phase was washed successively with 10% HCl and brine, dried and the solvent was removed in vacuo. The excess diethyl malonate was removed by distillation under reduced pressure. The resulting oil (15.6 g) was used without further purification.

1. temperaturethe resulting solution was heated
2. temperatureto reflux for 3 h
3. customEtOH was removed in vacuo
4. extractionextracted with Et2O
5. washThe organic phase was washed successively with 10% HCl and brine
6. customdried
7. customthe solvent was removed in vacuo
8. customThe excess diethyl malonate was removed by distillation under reduced pressure
9. customThe resulting oil (15.6 g) was used without further purification