HRID890739

反应详情

EQUATION

反应方程式

HRID 890739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4′-methyl-2-chloro-biphenyl (1.08 g, 5.33 mmol), NBS (1.14 g, 6.40 mmol) and AIBN (175 mg, 1.06 mmol) in CCl4 (37 mL) was heated at reflux for 3 h. The reaction mixture was diluted with CH2Cl2 and the organic solution was washed sequentially with aqueous saturated NaHCO3 (2×), water (1×), and brine (1×). The organic solution was dried over MgSO4, filtered, and concentrated in vacuo. The product was purified by flash chromatography (hexanes to 5% EtOAc/hexanes) to afford the title compound (920 mg). 1H NMR (CDCl3 400 MHz) δ 7.63–7.25 (m, 8H), 4.56 (s, 2H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 h
  3. washthe organic solution was washed sequentially with aqueous saturated NaHCO3 (2×), water (1×), and brine (1×)
  4. dry with materialThe organic solution was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe product was purified by flash chromatography (hexanes to 5% EtOAc/hexanes)