HRID1531810

反应详情

EQUATION

反应方程式

HRID 1531810 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Benzaldehyde-4-boronic acid (1.36 g), 2-bromo-4-cyano pyridine (1.5 g), cesium fluoride (2.72 g) and tetrakis(triphenylphosphine)palladium(0) (285 mg) were mixed together in dimethyl ethylene glycol (30 ml ). The reaction mixture was refluxed for 16 hrs under a atmosphere of nitrogen after which time the cooled mixture was diluted with diethyl ether (40 ml ) and washed with water (40 ml), the organic layer was separated and washed with saturated brine, dried over MgSO4 and evaporated under reduced pressure. The crude product was purified by column chromatography eluting with Dichloromethane/Diethyl ether (97.5/2.5, v/v) to afford the title compound (0.81 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 16 hrs under a atmosphere of nitrogen after which time the cooled mixture
  2. washwashed with water (40 ml)
  3. customthe organic layer was separated
  4. washwashed with saturated brine
  5. dry with materialdried over MgSO4
  6. customevaporated under reduced pressure
  7. customThe crude product was purified by column chromatography
  8. washeluting with Dichloromethane/Diethyl ether (97.5/2.5