反应详情

In 100 ml of ethanol was dissolved 4.2 g (1.1 eq.) of sodium, and a mixture of 25.0 g of 4-methoxyacetophenone and 27 ml (1.2 eq.) of diethyl oxalate was added dropwise under reflux. After 2 hours' reflux, the resulting crystals were collected by filtration. After 200 ml of 1N hydrochloric acid was added, the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off. The resulting crystals were collected by filtration with hexane.

1. additionwas added dropwise
2. temperatureunder reflux
3. temperatureAfter 2 hours' reflux
4. filtrationthe resulting crystals were collected by filtration
5. additionAfter 200 ml of 1N hydrochloric acid was added
6. extractionthe mixture was extracted with ethyl acetate
7. washThe organic layer was washed with water
8. dry with materiala saturated aqueous solution of sodium chloride and dried
9. distillationThe solvent was distilled off
10. filtrationThe resulting crystals were collected by filtration with hexane