HRID1036227
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 65 °C
PROCEDURE
实验过程
A mixture of diethyl 2-(2′,3-dimethyl-2,4′-bipyridin-5-yl)malonate 156-4 (935 mg, 3 mmol) and NaOH (480 mg, 12 mmol) in THF (1.8 mL) and water (1.8 mL) was stirred at 65° C. for 3 hours. After cooled down to room temperature, the mixture was treated with 3N HCl aqueous solution to adjust the pH around 3, and then stirred for 15 minutes. The resulting solution was evaporated to dryness and the remaining solid was extracted with 20% methanol in ethyl acetate. The organic extraction was concentrated to give 2-(2′,3-dimethyl-2,4′-bipyridin-5-yl)acetic acid 156-5 as white solid. MS m/z 243.1 (M+1).
WORKUP
后处理
- temperatureAfter cooled down to room temperature
- stirringstirred for 15 minutes
- customThe resulting solution was evaporated to dryness
- extractionthe remaining solid was extracted with 20% methanol in ethyl acetate
- extractionThe organic extraction
- concentrationwas concentrated