反应详情

58.5 g (1.08 mol) of sodium ethanolate are added to 500 ml of dimethyl carbonate. The mixture is then heated to boiling and traces of methanol are removed by distillation. 153.5 g (1.02 mol) of 2-methoxyacetophenone are allowed to drip in at 86° C. with vigorous stirring during the course of 4.5 hours. (If the reaction mixture becomes too viscous, a further addition of dimethyl carbonate is recommended.) The mixture is then subsequently stirred for a further 30 minutes and the solvent is removed by distillation under reduced pressure. After cooling to room temperature, 350 ml of water and 70 ml of glacial acetic acid are added and the mixture is stirred overnight. The oil formed is separated off and the aqueous phase is extracted by shaking with a total of 300 ml of ethyl acetate. The combined organic phases are first washed with a 6% strength sodium hydrogen carbonate solution (100 ml), then with a sodium chloride solution (the sodium chloride promotes the phase separation). After drying the ethyl acetate phase over sodium sulfate, filtration and after removing the solvent on a rotary evaporator, the remaining oil is distilled in a high vacuum.

1. temperatureThe mixture is then heated
2. customtraces of methanol are removed by distillation
3. customto drip in at 86° C.
4. stirring) The mixture is then subsequently stirred for a further 30 minutes
5. customthe solvent is removed by distillation under reduced pressure
6. addition350 ml of water and 70 ml of glacial acetic acid are added
7. stirringthe mixture is stirred overnight
8. customThe oil formed
9. customis separated off
10. extractionthe aqueous phase is extracted
11. stirringby shaking with a total of 300 ml of ethyl acetate
12. washThe combined organic phases are first washed with a 6% strength sodium hydrogen carbonate solution (100 ml)
13. customthe phase separation)
14. dry with materialAfter drying the ethyl acetate phase
15. filtrationover sodium sulfate, filtration
16. customafter removing the solvent
17. customon a rotary evaporator
18. distillationthe remaining oil is distilled in a high vacuum