HRID49131

反应详情

EQUATION

反应方程式

HRID 49131 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Tetrakis(triphenylphosphine)palladium (1 g) was added to a mixture of 5 g of 4-methoxyphenylboronic acid, 6.6 g of 5-bromo-2-fluoronitrobenzene and 30 mL of 2M sodium carbonate solution in 50 mL of toluene and 50 mL of ethanol. The mixture was heated to reflux for 2 hours, concentrated, and the residue extracted twice with ethyl acetate. The ethyl acetate layer was washed with water, brine, dried, and concentrated to give a brown oily solid. The solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane to give crude-4-fluoro-4′-methoxy-3-nitrobiphenyl as a pale yellow solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 2 hours
  3. concentrationconcentrated
  4. extractionthe residue extracted twice with ethyl acetate
  5. washThe ethyl acetate layer was washed with water, brine
  6. customdried
  7. concentrationconcentrated
  8. customto give a brown oily solid
  9. customThe solid was purified by column chromatography on silica gel in 5% ethyl acetate in hexane