HRID36818

反应详情

EQUATION

反应方程式

HRID 36818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a mixture of 4.2 g of the 4-bromo-1-n-octyloxybenzene, 0.5 g of tetrakis(triphenylphosphine) palladium(0), 53 ml of benzene, and 53 ml of an aqueous sodium carbonate solution (2 mol/liter), 26 ml of ethanol containing 3.0 g of 2,3-difluorophenyl boronic acid synthesized by the same method as in [1] in Example 1 was added dropwise, and then the solution thus formed was heated to reflux for 5 hours. After the solution was cooled, it was added with 200 ml of an ether to extract the product, washed with water and dried. The solvent was distilled off under a reduced pressure. The residue thus obtained was purified by a silica gel column chromatography using a mixed solvents of n-hexane and diethyl ether (10:2) to obtain 2.8 g of 4-n-octyloxy-2', 3'-difluorobiphenyl.

WORKUP

后处理

  1. additionwas added dropwise
  2. customthe solution thus formed
  3. temperaturewas heated
  4. temperatureto reflux for 5 hours
  5. temperatureAfter the solution was cooled
  6. extractionto extract the product
  7. washwashed with water
  8. customdried
  9. distillationThe solvent was distilled off under a reduced pressure
  10. customThe residue thus obtained
  11. customwas purified by a silica gel column chromatography