反应详情

Diethyl malonate (73. 7 g) was dissolved in ethanol (700 ml), and then potassium tert-butoxide (51.6 g) was gradually added thereto. A solution of 4-(3,4-dimethoxyphenyl)-3-buten-2-one (79.1 g) in ethanol (500 ml) was added dropwise, and the mixture was refluxed for 1.5 hours. After distilling off the reaction solvent under reduced pressure, ice water was poured over it and it was adjusted to pH4 with concentrated hydrochloric acid. The deposited crystals were filtered by suction, washed with water and then air-dried to give 122 g of ethyl 2-(3,4-dimethoxyphenyl)-4,6-dioxocyclohexane carboxylate (99.6%).

1. temperaturethe mixture was refluxed for 1.5 hours
2. distillationAfter distilling off the reaction solvent under reduced pressure, ice water
3. additionwas poured over it and it
4. filtrationThe deposited crystals were filtered by suction
5. washwashed with water
6. customair-dried