HRID931137
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
PROCEDURE
实验过程
To a solution of 3-bromo-5-cyanopyridine (1 g, 5.3 mmol) in tetrahydrofuran was added cyclopropyl boronic acid (0.5 g, 5.6 mmol) and potassium phosphate (1.08 g, 15.9 mmol). The resulting solution was degassed with nitrogen for 10 minutes and then palladium (II) acetate and S-phos were added. The reaction mixture was refluxed for 16 h. The reaction mixture was diluted with water, extracted with ethyl acetate and concentrated under reduced pressure. The crude material was purified via column chromatography to afford 5-cyclopropylnicotinonitrile (0.45 g, 58%). MS (ES+) (M+H) 145.1774.
WORKUP
后处理
- customThe resulting solution was degassed with nitrogen for 10 minutes
- additionpalladium (II) acetate and S-phos were added
- temperatureThe reaction mixture was refluxed for 16 h
- additionThe reaction mixture was diluted with water
- extractionextracted with ethyl acetate
- concentrationconcentrated under reduced pressure
- customThe crude material was purified via column chromatography