HRID415289

反应详情

EQUATION

反应方程式

HRID 415289 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of 3-boronobenzoic acid (1.66 g, 10 mmol) and 2-bromopyridine (1.72 g, 11 mmol) in acetonitrile (40 mL) and water (40 mL), potassium carbonate (5.5 g, 40 mmol), Bis(triphenylphosphine)palladium(II)chloride (400 mg, 0.37 mmol) was added. The mixture was degassed and purged withed nitrogen. The mixture was stirred at 100° C. for 24 h. Then the hot suspension was filtered and concentrated to half of the original volume and washed with dichloromethane. The aquatic phase was adjusted to pH=3 with hydrochloric acid (1 M) and filtrated, washed with water. The residue was dried in vacuum to obtain 1.69 g of white solid of 3-(pyridin-2-yl)benzoic acid. Yield: 85%. LC-MS (ESI) m/z: 200 (M+1)+.

WORKUP

后处理

  1. customThe mixture was degassed
  2. custompurged
  3. filtrationThen the hot suspension was filtered
  4. concentrationconcentrated to half of the original volume
  5. washwashed with dichloromethane
  6. filtrationfiltrated
  7. washwashed with water
  8. customThe residue was dried in vacuum