反应详情

39.3 g of sodium tert-butylate (0.41 mol) were introduced as initial charge in 300 ml of dioxane, and 65.5 g of diethyl malonate (0.41 mol) were added dropwise over the course of 15 min such that the temperature does not exceed 30° C. After 1 h, 2.70 g (8.8 mmol) of bis(2-pyridinecarboxylato)copper(II) complex and 38.0 g (0.12 mol) of 3-bromo-1-(2-methoxy-4-nitrophenyl)pyridin-2(1H)-one were added and the reaction mixture was heated at reflux for 8 h. After cooling to RT, the mixture was further stirred overnight. The reaction mixture was filtered off from the solid with suction, the residue was after-washed with dioxane and the combined organic fractions were evaporated to ca. 300 g on a rotary evaporator. The crude solution was used in the next stage without further purification.

1. customdoes not exceed 30° C
2. temperaturethe reaction mixture was heated
3. temperatureat reflux for 8 h
4. waitthe mixture was further stirred overnight
5. filtrationThe reaction mixture was filtered off from the solid with suction
6. washthe residue was after-washed with dioxane
7. customthe combined organic fractions were evaporated to ca. 300 g on a rotary evaporator
8. customThe crude solution was used in the next stage without further purification