反应详情

温度

60 °C

20.6 g of thiourea were suspended in 900 ml of dry ethanol, and 75 ml of sodium methoxide solution (30% in methanol) were added. After 15 min, 91.0 g of diethyl 2-(4-methoxy-3,5-dimethylbenzoylamino)malonate were added a little at a time. Initially, this gave a clear solution, and soon a pale-yellow precipitate was formed. The reaction was then stirred at 60° C. for 3 hours. At room temperature, the precipitated solid was filtered off with suction and washed with about 100 ml of ethanol and then with diethyl ether, and dried under reduced pressure. This gave 78.3 g (84%) of the title compound which was reacted further without any further purification.

1. customInitially, this gave a clear solution
2. customsoon a pale-yellow precipitate was formed
3. filtrationAt room temperature, the precipitated solid was filtered off with suction
4. washwashed with about 100 ml of ethanol
5. dry with materialwith diethyl ether, and dried under reduced pressure
6. customThis gave 78.3 g (84%) of the title compound which was reacted further without any further purification