HRID369245

反应详情

EQUATION

反应方程式

HRID 369245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Sodium methoxide (28% methanol solution; 1.66 g) was added to a solution of methyl 2,5-difluoro-3-methyl-4-nitrobenzoate (1.0 g) in acetonitrile (5 ml) under ice cooling, and the mixture was stirred for 1 hour at 0° C. and for 2 hours at 50° C. The reaction mixture was additionally stirred overnight at room temperature and then poured into ice water. The mixture was acidified with citric acid and then extracted with diethyl ether. An organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Diethyl ether was added to the residue, and insoluble matter was removed by filtration. The filtrate was concentrated under reduced pressure to obtain the title compound (1.1 g).

WORKUP

后处理

  1. waitThe reaction mixture was additionally stirred overnight at room temperature
  2. extractionextracted with diethyl ether
  3. dry with materialAn organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionDiethyl ether was added to the residue, and insoluble matter
  6. customwas removed by filtration
  7. concentrationThe filtrate was concentrated under reduced pressure