反应详情

7.1 g of sodium methoxide was added to 100 ml of dry ether, and the mixture was stirred. A solution of 20 g of ethyl chlorodifluoroacetate diluted with 25 ml of dry ether was added dropwise at room temperature. Further, a solution of 12.5 g of pinacolone diluted with 25 ml of dry ether was added dropwise, and the mixture was stirred overnight at room temperature. Then, to the reaction solution, a solution of 8.4 g of glacial acetic acid diluted with 100 ml of water and a solution of 23.6 g of copper (II) acetate dissolved in a proper amount of water were added dropwise successively. The dropwise addition was followed by stirring for about 10 minutes. Then, the ether was distilled off under reduced pressure and the solid mass was filtered off. After vacuum drying, 100 ml of 6N hydrochloric acid was added, and extraction with ethyl acetate was carried out. The ethyl acetate layer was dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. Then, the residue was subjected to vacuum distillation to obtain 13 g of the desired product. (b.p. 54°-57° C./5 mmHg)

1. additionwas added dropwise at room temperature
2. additionwas added dropwise
3. stirringthe mixture was stirred overnight at room temperature
4. additionwere added dropwise successively
5. additionThe dropwise addition
6. stirringby stirring for about 10 minutes
7. distillationThen, the ether was distilled off under reduced pressure
8. filtrationthe solid mass was filtered off
9. customAfter vacuum drying
10. addition100 ml of 6N hydrochloric acid was added
11. extractionextraction with ethyl acetate
12. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
13. distillationthe solvent was distilled off under reduced pressure
14. distillationThen, the residue was subjected to vacuum distillation