HRID488498

反应详情

EQUATION

反应方程式

HRID 488498 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of sodium metal (1.27 g, 0.055 mol) and MeOH (250 mL) was stirred at 0° C. for 10 minutes. This solution was added to a solution of 2-fluoro-5-nitrobenzoic acid methyl ester (10.0 g, 0.046 mol) in MeOH (250 mL), and the mixture was stirred for 20 minutes at 0° C. to 5° C. The reaction mixture was then allowed to warm to room temperature and stir for 2 hours. The mixture was then filtered to give an off-white precipitate. Recrystallization with CHCl3 (70 ml) yielded an off-white crystalline solid, 1.825 g (0.008 mol, 17%) of the title compound.

WORKUP

后处理

  1. stirringthe mixture was stirred for 20 minutes at 0° C. to 5° C
  2. temperatureto warm to room temperature
  3. stirringstir for 2 hours
  4. filtrationThe mixture was then filtered
  5. customto give an off-white precipitate
  6. customRecrystallization with CHCl3 (70 ml)