HRID505123

反应详情

EQUATION

反应方程式

HRID 505123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (commercially available) (1-bromo-2-trifluoromethoxy-benzene) in DME (first degased with argon) under argon was added 3 mol % Pd(PPh3)4, pyridyl-4-boronic acid and 2N Na2CO3, the resulting reaction mixture was vigorously stirred under reflux. After 5 h at reflux, reaction as monitored by TLC showed completion. Two phases were separated, evaporation of most of the DME, redissolution of the residue in EtOAc and washing with aq. NaOH followed by evaporation gave a yellow oil. Flash Chromatography on SiO2 gel with a mixture of CH2Cl2/MeOH gave the title compound in 51% yield.

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. temperatureunder reflux
  3. temperatureAfter 5 h at reflux
  4. customreaction
  5. customTwo phases were separated
  6. customevaporation of most of the DME, redissolution of the residue in EtOAc
  7. washwashing with aq. NaOH
  8. customfollowed by evaporation
  9. customgave a yellow oil