反应详情

Diethyl aminomalonate hydrochloride (20.5 g) was suspended into 180 ml of methylene chloride, and 29.4 g of triethylamine was added while cooling with ice-cold water. After 30-minute-stirring, 15 g of p-toluoyl chloride was added dropwise, and the mixture was stirred for 24 hours at room temperature. The reaction solution was washed with water, dilute hydrochloric acid, and water, dried over anhydrous magnesium sulfate and concentrated. To the residue was added isopropyl ether, and the resultant crystals were collected by filtration and dried to provide 25.9 g of the objective compound as white crystal. M.p. 101-102° C.

1. additionwas added
2. temperaturewhile cooling with ice-cold water
3. stirringthe mixture was stirred for 24 hours at room temperature
4. washThe reaction solution was washed with water, dilute hydrochloric acid, and water
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. additionTo the residue was added isopropyl ether
8. filtrationthe resultant crystals were collected by filtration
9. customdried