反应详情

A solution of 2.6 g (0.1124 g-atom) of Na in 50 mL of MeOH was treated with 12.9 mL (0.1124 mol) of dimethyl malonate and allowed to stir for 45 minutes. This was then treated dropwise with 24.17 g (0.1124 mol) of 3-methoxy-4-methylbenzyl bromide and the solution heated at reflux overnight. The solvent was removed under reduced pressure and the residue taken up in EtOAc. This was washed with 6% HCl, H2O, saturated NaHCO3, and saturated NaCl. Drying over MgSO4 and removal of the solvent under reduced pressure gave 28.54 g (95.5% yield) of the product as a pale yellow oil. The structure was confirmed by NMR spectroscopy.

1. temperaturethe solution heated
2. temperatureat reflux overnight
3. customThe solvent was removed under reduced pressure
4. washThis was washed with 6% HCl, H2O, saturated NaHCO3, and saturated NaCl
5. dry with materialDrying over MgSO4 and removal of the solvent under reduced pressure