反应详情

116.8 g of diethyl aminomalonate hydrochloride were dissolved in 700 ml of dichloromethane, and 231 ml of triethylamine were added with cooling in an ice bath. A solution of 109.6 g of 4-methoxy-3,5-dimethylbenzoyl chloride in 400 ml of dichloromethane was then slowly added dropwise. After 2 h at 0° C., 200 ml of water were added slowly. After phase separation, the aqueous phase was extracted twice with 200 ml of dichloromethane. The combined organic phases were washed with 2M hydrochloric acid and then with water, dried with sodium sulfate, filtered and evaporated. The residue was treated with methyl tert-butyl ether, after which the precipitate obtained was filtered off, which gave 178.7 g of the title compound.

1. temperaturewith cooling in an ice bath
2. customAfter phase separation
3. extractionthe aqueous phase was extracted twice with 200 ml of dichloromethane
4. washThe combined organic phases were washed with 2M hydrochloric acid
5. dry with materialwith water, dried with sodium sulfate
6. filtrationfiltered
7. customevaporated
8. additionThe residue was treated with methyl tert-butyl ether
9. customafter which the precipitate obtained
10. filtrationwas filtered off