反应详情

温度

100 °C

2-(6-Bromo-pyridin-2-yl)-malonic acid diethyl ester (64.0 g, 202.4 mmol) was added to a solution of potassium carbonate (279.8 g, 2024 mmol) in water (400 ml) at rt and the reaction mixture was heated to reflux at 100° C. for 36 h. The reaction mixture was treated with sat. ammonium chloride solution and the product formed was extracted with ethyl acetate (3×800 ml), washed with brine (10 ml). Organic layer was concentrated under reduced pressure to obtain title compound as a pale brown solid. Yield=34.0 g (77.7%). TLC (50% ethyl acetate in hexane) Rf=0.11; LCMS: RtH8=0.45; [M+1]=216.0 and 218.0.

1. temperaturethe reaction mixture was heated
2. customthe product formed
3. extractionwas extracted with ethyl acetate (3×800 ml)
4. washwashed with brine (10 ml)
5. concentrationOrganic layer was concentrated under reduced pressure