HRID1487213

反应详情

EQUATION

反应方程式

HRID 1487213 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

A mixture of 7-nitrobenzofuran-2-carboxylic acid (3.54 g, 17.1 mmol) and copper(II) oxide (0.16 g, 2 mmol) in quinoline (30 mL) was heated at 170° C. for 1 hour. Cooling to room temperature, the mixture was diluted with water and extracted with ethyl acetate. The combined organic extracts were washed by brine, dried over anhydrous sodium sulfate, evaporated and purified by silica gel chromatography (petroleum ether/dichloromethane 2/3) to afford the product 7-nitrobenzofuran (2.56 g, yield 92%). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.27-8.28 (d, 1H, J=2.0 Hz), 8.12-8.17 (m, 2H), 7.46-7.50 (t, 1H, J=8.0 Hz), 7.215-7.220 (d, 1H, J=2.0 Hz).

WORKUP

后处理

  1. temperatureCooling to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe combined organic extracts were washed by brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. custompurified by silica gel chromatography (petroleum ether/dichloromethane 2/3)