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25.7 g (1.1 mol eq.) of sodium in small pieces were added gradually to a solution of 198 g (1.1 mol) of homoveratronitrile in 500 ml of diethyl carbonate in such a manner that the temperature remained at approximately 100°. Thereafter, the reaction mixture was heated to reflux for 1 hour, evaporated under reduced pressure, treated with cooled water, acidified with 70 ml of glacial acetic acid and extracted with ether. The combined organic extracts were dried and evaporated. The residual oil was distilled in a high vacuum, whereby ethyl 3,4-dimethoxyphenylcyanoacetate was obtained, b.p. 170°-172°/70 Pa. HPLC purity >99%.

1. customremained at approximately 100°
2. temperatureThereafter, the reaction mixture was heated
3. temperatureto reflux for 1 hour
4. customevaporated under reduced pressure
5. additiontreated with cooled water
6. extractionextracted with ether
7. customThe combined organic extracts were dried
8. customevaporated
9. distillationThe residual oil was distilled in a high vacuum