HRID1842987

反应详情

EQUATION

反应方程式

HRID 1842987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

To a solution of ethyl 2-(4-(ethylsulfonamidomethyl)-3-fluorophenyl)propanoate (305 mg, 1.03 mmol) in DMF, manganese (113 mg, 2.06 mmol), NiBr2bipy (27 mg, 0.07 mmol), ethyl-2-chloro propionate (0.17 mL, 1.34 mmol) was added, followed by addition of TFA (0.002 mL, 0.028 mmol). The mixture was stirred for 1 day at 65° C. The reaction mixture was quenched by conc. HCl (7-drops) and then extracted with diethyl ether, dried (MgSO4) and the solvent was evaporated in vacuo. The residue was purified by CC (EtOAc/n-hexane). 2-(4-(ethyl-sulfonamidomethyl)-3-fluorophenyl)propanoic acid in pure form (65 mg, 20%) was obtained.

WORKUP

后处理

  1. customThe reaction mixture was quenched by conc. HCl (7-drops)
  2. extractionextracted with diethyl ether
  3. dry with materialdried (MgSO4)
  4. customthe solvent was evaporated in vacuo
  5. customThe residue was purified by CC (EtOAc/n-hexane)