HRID536175

反应详情

EQUATION

反应方程式

HRID 536175 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 4-(bromomethyl)-1-chloro-2-(trifluoromethyl)benzene (4.5 g, 16.45 mmol), potassium trifluoro(4-formylphenyl)borate (3.52 g, 16.62 mmol), PdCl2(dppf)-CH2Cl2 adduct (0.672 g, 0.823 mmol) and Cs2CO3 (16.08 g, 49.4 mmol) in cyclopentyl methyl ether (100 mL) and water (100 mL). The mixture was charged with Argon and stirred for overnight at 80° C. The result mixture was cooled to room temperature and partitioned with water 100 mL and ethyl acetate 100 mL. The organic phase was washed by water, brine and dried over sodium sulfate, the solvent was removed and the residue was purified via flash column chromatography. Removed the solvent afforded the title compound (2.55 g). LC-MS (ESI): m/z 299 [M+H]+

WORKUP

后处理

  1. additionThe mixture was charged with Argon
  2. temperatureThe result mixture was cooled to room temperature
  3. custompartitioned with water 100 mL and ethyl acetate 100 mL
  4. washThe organic phase was washed by water, brine
  5. dry with materialdried over sodium sulfate
  6. customthe solvent was removed
  7. customthe residue was purified via flash column chromatography
  8. customRemoved the solvent