HRID1443828

反应详情

EQUATION

反应方程式

HRID 1443828 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the solution of (2,3-dihydro-benzofuran-5-yl)-acetic acid (0.89 g, 5 mmol) and N-bromosuccinimide (0.89 g, 5 mmol) in carbon tetrachloride (10 mL) was added 10 mg of benzoyl peroxide. The mixture was refluxed for 3 h and cooled with ice. The solid was removed by filtration, the filtrate was concentrated, the residue was crystallized from 1:1 ethyl acetate:hexane to give a white solid (390 mg, 44%). 1H NMR (400 MHz, CDCl3) δ 10.5 (b s, 1H), 7.62 (d, J=2.2 Hz, 1H), 7.52 (d, J=1.4 Hz, 1H), 7.46 (d, J=8.4 Hz, 1H), 7.21 (dd, J=8.4, 1.8 Hz, 1H), 6.74 (d, J=2.2 Hz, 1H), 3.75 (s, 2H).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 3 h
  2. temperaturecooled with ice
  3. customThe solid was removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customthe residue was crystallized from 1:1 ethyl acetate