HRID1057451

反应详情

EQUATION

反应方程式

HRID 1057451 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 2 M sodium carbonate solution in 50 mL of toluene and 50 mL of ethanol. The mixture was heated to refulux 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 chromatographed 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. concentrationconcentrated
  3. extractionthe residue extracted twice with ethyl acetate
  4. washThe ethyl acetate layer was washed with water, brine
  5. customdried
  6. concentrationconcentrated
  7. customto give a brown oily solid
  8. customThe solid was chromatographed on silica gel in 5% ethyl acetate in hexane