HRID449093

反应详情

EQUATION

反应方程式

HRID 449093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-bromo-3-chlorophenol (2.0 g, 0.0096 mol), phenylboronic acid (3.5 g, 0.029 mol), TEA (8.1 mL, 0.058 mol), cupric acetate (3.2 g, 0.017 mol) and DCM (40 mL) were added to a 100 mL oven dried flask and the reaction was stirred at rt for 24 h. Reaction mixture was then filtered through celite. The filtrate was concentrated in vacuo to give a residue which was purified by silica gel chromatography, eluting with 5% EtOAc in hexane. 1H NMR (400 MHz, CDCl3): δ=6.74 (dd, J=8.84, 2.78 Hz, 1H), 6.94-7.02 (m, 2H), 7.06 (d, J=2.78 Hz, 1H), 7.14 (t, J=7.33 Hz, 1H), 7.29-7.38 (m, 2H), 7.48 (d, J=8.84 Hz, 1H).

WORKUP

后处理

  1. customdried flask
  2. customReaction mixture
  3. filtrationwas then filtered through celite
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto give a residue which
  6. customwas purified by silica gel chromatography
  7. washeluting with 5% EtOAc in hexane