反应详情

温度

93 °C

30.7 g of sodium was added to 300 ml of toluene, and the mixture was heated to 93° C., followed by cooling while vigorous stirring, to give sandy products. To the product, 600 ml of toluene containing 300 g of dimethyl carbonate was added, and further 250 ml of a toluene solution containing 100 g of p-methoxyacetophenone was added dropwise over 2 hours and 15 minutes at 84° to 86° C. After the dropwise addition, the mixture was stirred under heating at 82° to 83° C. for 1.5 hours, and then the solvent was evaporated. To the residue was added 1 l of isopropyl ether, and crystals were collected by filtration and washed with 500 ml of isopropyl ether. These crystals were added to a mixture of ice and ethyl acetate containing 100 g of acetic acid, and extracted with ethyl acetate. The extract was washed with 5 % sodium hydrogen carbonate and then with water, and dried. Subsequently, the solvent was evaporated to obtain 131.6 g of methyl 3-oxo-3-(p-methoxyphenyl)propionate as an oily product.

1. temperatureby cooling while vigorous stirring
2. customto give sandy products
3. additionwas added dropwise over 2 hours and 15 minutes at 84° to 86° C
4. additionAfter the dropwise addition
5. temperatureunder heating at 82° to 83° C. for 1.5 hours
6. customthe solvent was evaporated
7. additionTo the residue was added 1 l of isopropyl ether, and crystals
8. filtrationwere collected by filtration
9. washwashed with 500 ml of isopropyl ether
10. additionThese crystals were added to a mixture of ice and ethyl acetate containing 100 g of acetic acid
11. extractionextracted with ethyl acetate
12. washThe extract was washed with 5 % sodium hydrogen carbonate
13. dry with materialwith water, and dried
14. customSubsequently, the solvent was evaporated