HRID453676

反应详情

EQUATION

反应方程式

HRID 453676 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) was dissolved in aniline (25 ml, 274 mmol), and the mixture reacted in a closed vessel under microwave irradiation at 120° C. for 5 minutes (UPLC-MS monitoring: complete conversion). Dichloromethane (DCM) (100 ml) was added to the reaction mixture, and the resulting solid was filtered; 2M Na2CO3 (50 ml) was added to the solution, and the aqueous layer was washed with DCM (3×100 ml). The aqueous layer was acidified with 12N HCl (36 ml) and the title compound was recovered as racemic mixture by filtration (5.1 g, 97% yield).

WORKUP

后处理

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