Diethyl Malonate → HCID 68209677, compound

Participants

Reaction Conditions

Reaction Steps

Under argon, 42.5 g (379 mmol) of potassium tert-butylate were suspended in 530 ml of dioxane and heated to 55-60° C. At this temperature, a solution of 60.7 g (379 mmol) of diethyl malonate in 100 ml of dioxane was added over 20 min. When the addition was complete, the reaction mixture was stirred for 1 h at 60° C. 6.72 g (21.7 mmol) of bis(2-pyridinecarboxylato)copper(II) complex were then added, as were 35.0 g (108 mmol) of 3-bromo-1-(2,6-dimethyl-4-nitrophenyl)pyridin-2(1H)-one. The reaction mixture was heated at reflux for 8 h and then stirred overnight at RT. Filtering off the liquid from the solid with suction was carried out, followed by after-washing with dioxane, and the filtrate was evaporated to 250 g on a rotary evaporator. The crude solution was further reacted without purification.

Provenance & Evidence