反应详情

58.4 g of diethyl aminomalonate hydrochloride were suspended in 300 ml of dichloromethane, and 115 ml of triethylamine were added with ice cooling. At 0° C., 54.8 g of 4-methoxy-3,5-dimethylbenzoyl chloride in 250 ml of dichloromethane were then added dropwise. After 2 hours at 0° C., 100 ml of water were added dropwise, and the aqueous phase was separated off and extracted with 200 ml of dichloromethane. The combined organic phases were extracted first with 2M aqueous hydrochloric acid and then with water, dried over sodium sulfate, filtered and concentrated. The residue was triturated with methyl tert-butyl ether, filtered off with suction and dried under reduced pressure. This gave 89.3 g (96%) of the title compound which was reacted further without any further purification.

1. customthe aqueous phase was separated off
2. extractionextracted with 200 ml of dichloromethane
3. extractionThe combined organic phases were extracted first with 2M aqueous hydrochloric acid
4. dry with materialwith water, dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was triturated with methyl tert-butyl ether
8. filtrationfiltered off with suction
9. customdried under reduced pressure
10. customThis gave 89.3 g (96%) of the title compound which was reacted further without any further purification