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
- 80 °C
PROCEDURE
实验过程
To a solution of methyl 3-bromo-5-(5-methylpyridin-2-yl)benzoate (1.00 g, 3.27 mmol) in N,N-dimethylformamide (9.80 mL) and water (3.27 mL) was 2-isopropenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.921 mL, 4.90 mmol), palladium(II) acetate (37.0 mg, 0.163 mmol), 3,3′3″-phosphinidynetris(benzenesulfonic acid)trisodium salt (278 mg, 0.490 mmol) and diisopropylamine (1.16 mL, 8.17 mmol) and the mixture was heated to 80° C. After 50 min, the reaction was allowed to cool to ambient temperature and filtered. Purification by reverse phase chromatography (C-18, 90% water/acetonitrile→40% water/acetonitrile with 0.1% trifluoroacetic acid) gave the title compound (864 mg). MS 268.2 (M+1).
WORKUP
后处理
- temperatureto cool to ambient temperature
- filtrationfiltered
- customPurification by reverse phase chromatography (C-18, 90% water/acetonitrile→40% water/acetonitrile with 0.1% trifluoroacetic acid)