HRID1492302

反应详情

EQUATION

反应方程式

HRID 1492302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Bromosuccinimide (6.64 g) and azo(bisisobutyronitrile) (400 mg) were added to a solution of compound (B) (10.1 g) in carbon tetrachloride (100 ml). The mixture was heated under reflux for 20 hours and then cooled to ambient temperature. Insoluble material was removed by filtration and the filtrate was concentrated. The residue was purified by flash chromatography eluting with ethyl acetate/hexane (1:19 v/v), to give ethyl 2-(4-bromomethylphenoxy)phenylacetate (C) (5.9 g), as an oil; NMR (d6 -DMSO): 1.15(t, 3H), 4.1(q, 2H), 4.65(s, 2H), 6.0(s, 1H), 6.95(d, 2H), 7.3-7.5(m, 5H), 7.5-7.6(m, 2H).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 20 hours
  3. customInsoluble material was removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by flash chromatography
  6. washeluting with ethyl acetate/hexane (1:19 v/v)