HRID639844

反应详情

EQUATION

反应方程式

HRID 639844 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

[(3-Bromo-3-buten-1-yl)oxy](1,1-dimethylethyl)diphenylsilane (P12, 3.50 g) and (3,4-dichlorophenyl)boronic acid (2.06 g) were dissolved in toluene (45 mL), the stirred solution was degassed, then tetrakis(triphenylphosphine)palladium(0) (0.363 g) and ethanol (33 mL) were added and the mixture was degassed again. A 2N aqueous solution of Na2CO3 (24 mL) was added and the mixture was heated to 80° C. and stirred under nitrogen atmosphere for 3 h at this temperature. After cooling to RT, the reaction mixture was extracted with ethyl ether, the organic phase was washed with brine, dried over Na2SO4 and the solvent removed under reduced pressure. The crude product was purified by flash chromatography (eluting with cy/EA from 100/0 to 95/5) to give the title compound (2.65 g) as a colourless oil.

WORKUP

后处理

  1. customthe stirred solution was degassed
  2. additiontetrakis(triphenylphosphine)palladium(0) (0.363 g) and ethanol (33 mL) were added
  3. customthe mixture was degassed again
  4. additionA 2N aqueous solution of Na2CO3 (24 mL) was added
  5. temperatureAfter cooling to RT
  6. extractionthe reaction mixture was extracted with ethyl ether
  7. washthe organic phase was washed with brine
  8. dry with materialdried over Na2SO4
  9. customthe solvent removed under reduced pressure
  10. customThe crude product was purified by flash chromatography (eluting with cy/EA from 100/0 to 95/5)