HRID1171502

反应详情

EQUATION

反应方程式

HRID 1171502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux for 48 h
  3. temperatureAfter cooling
  4. addition1N HCL was added
  5. customA white precipitate was formed
  6. customwas removed by filtration
  7. customA small portion of the filtrate was purified by reverse phase HPLC (gradient elution, water/acetonitrile/TFA)