HRID1171502
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
6-Bromopicolinic acid (1.0 g) was dissolved in 1,2-dimethoxyethane (15 mL) prior to the addition of palladium tetrakistriphenylphoshine (572 mg), 2M Na2CO3 (5 mL), and phenyl boronic acid (905 mg). The resulting solution was heated at reflux for 48 h. After cooling, 1N HCL was added to adjust the pH<4. A white precipitate was formed and was removed by filtration. A small portion of the filtrate was purified by reverse phase HPLC (gradient elution, water/acetonitrile/TFA) to afford 6-phenylpicolinic acid (25 mg). MS found: (M+H)+=200.1.
WORKUP
后处理
- temperatureThe resulting solution was heated
- temperatureat reflux for 48 h
- temperatureAfter cooling
- addition1N HCL was added
- customA white precipitate was formed
- customwas removed by filtration
- customA small portion of the filtrate was purified by reverse phase HPLC (gradient elution, water/acetonitrile/TFA)