反应详情

To a mixture of 5.15 g of ethyl 2-(p-formylphenyl)propionate and 4.2 g of cycloheptanone were added dropwise at room temperature 30 ml of an aqueous solution of 2.6 g of sodium hydroxide and the resulting mixture was heated under reflux for 3 hours. After cooling, the reaction mixture was extracted twice with ethyl acetate, an aqueous layer was made acidic with hydrochloric acid and extracted with ethyl acetate. The extract was washed with water and dried over anhydrous sodium sulfate. The ethyl acetate was distilled off to leave an oily substance, which was then subjected to a silica gel column chromatography and elution was effected with benzene-ethyl acetate 5:1 to yield an yellow oily substance. The substance was distilled under reduced pressure to give 2.7 g of the desired product as a pale yellow oily substance having a boiling point of 210°-215° C./0.3 mmHg (bath temp.).

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 3 hours
3. temperatureAfter cooling
4. extractionthe reaction mixture was extracted twice with ethyl acetate
5. extractionextracted with ethyl acetate
6. washThe extract was washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe ethyl acetate was distilled off
9. customto leave an oily substance, which
10. washwas then subjected to a silica gel column chromatography and elution
11. customto yield an yellow oily substance
12. distillationThe substance was distilled under reduced pressure