HRID76963

反应详情

EQUATION

反应方程式

HRID 76963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

α-Bromophenylacetic acid (5.01 g, 23.2 mmol.) is dissolved in aniline (25 mL, 274 mmol) and the mixture reacted in a closed vessel under MW irradiation at 120° C. for 5 minutes (LC-MS monitoring: complete conversion). Dichloromethane (DCM) (100 mL) is added to the reaction mixture and the resulting solid is filtered; 2M Na2CO3 (50 mL) is added to the solution, and the aqueous layer is washed with DCM (3×100 mL). The aqueous layer is acidified with 12N HCl (36 mL), and the title compound is recovered as racemic mixture by filtration (5.1 g, 97% yield, white solid).

WORKUP

后处理

  1. customthe mixture reacted in a closed vessel under MW irradiation at 120° C. for 5 minutes (LC-MS monitoring: complete conversion)
  2. filtrationthe resulting solid is filtered
  3. addition2M Na2CO3 (50 mL) is added to the solution
  4. washthe aqueous layer is washed with DCM (3×100 mL)
  5. filtrationthe title compound is recovered as racemic mixture by filtration (5.1 g, 97% yield, white solid)