HRID76454

反应详情

EQUATION

反应方程式

HRID 76454 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 2-carboxy-5-nitrobenzofuran (2.0 g), MeOH (10 mL) and Concentrated H2SO4 (2.1 mL) was heated in a sealed tube at 60° C. for 3 h. Upon cooling to the room temperature it was quenched with ice-water and carefully basified with addition of NaHCO3. The solid obtained was filtered, washed with water, dried and analyzed to give 2-methoxycarbonyl-5-nitrobenzofuran. 1H NMR (CDCl3): δ 8.66 (d, 1H, J=2.4 Hz), 8.36 (dd, 1H, J=2.4 and 9.6 Hz), 7.71 (d, 1H, J=9.3 Hz), 7.65 (s, 1H), 4.01 (s, 3H); LCMS: purity: 97%; MS (m/e): 222 (MH+).

WORKUP

后处理

  1. temperatureUpon cooling to the room temperature it
  2. customwas quenched with ice-water
  3. additioncarefully basified with addition of NaHCO3
  4. customThe solid obtained
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried