HRID59240

反应详情

EQUATION

反应方程式

HRID 59240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-chloro-5-nitrobenzoic acid (3.0 g, 0.14 mol) in methanol (500 mL) was added sodium methoxide (28.1 g, 0.520 mol). The reaction mass was refluxed for 15 h. Excess of solvent was removed under vacuum and the reaction mass was diluted with water and acidified with dilute HCl to obtain solid which was filtered off to afford 25.0 g of desired product. 1H NMR (300 MHz, DMSO d6): δ 3.96 (s, 3H), 7.36 (d, J=9.3 Hz, 1H), 8.37 (d, J=9.0 Hz, 1H), 8.45 (s, 1H), 13.32 (br s, 1H)); MS (m/z): 198.25 (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mass was refluxed for 15 h
  2. customExcess of solvent was removed under vacuum
  3. additionthe reaction mass was diluted with water
  4. customto obtain solid which
  5. filtrationwas filtered off