HRID38159

反应详情

EQUATION

反应方程式

HRID 38159 的结构方程式

PROCEDURE

实验过程

To a chilled solution of 2-amino-4-fluorobenzoic acid (1.57 g, 10.1 mmol) in absolute ethanol (20 mL) was added neat thionyl chloride (4.4 mL, 60 mmol). The reaction mixture was refluxed for 4 days total, with addition of more SOCl2 (8 mL, 110 mmol), then concentrated, diluted with EtOAc, washed with 2N NaOH, dried and concentrated in vacuo to give ethyl 2-amino-4-fluorobenzoate (1.73 g, 94%).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 4 days total
  2. concentrationconcentrated
  3. additiondiluted with EtOAc
  4. washwashed with 2N NaOH
  5. customdried
  6. concentrationconcentrated in vacuo