HRID1771749

反应详情

EQUATION

反应方程式

HRID 1771749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-fluoro-3-[[2-fluoro-5-(3-fluorophenyl)-3-methyl-phenyl]methyl amino]-2-methyl-phenol (269 mg, 0.8 mmol, 1 eq), in 2-butanone (10 mL) was added Cs2CO3 (368 mg, 0.9 mmol, 1.5 eq) and isopropyl 2-bromoacetate (163.5 mg, 0.9 mmol, 1.2 eq). The reaction mixture was stirred at room temperature for 2 h, then filtered to remove the solids. The filtrate was evaporated in vacuo and the crude residue obtained purified by column chromatography (petroleum ether:EtOAc, 100:1 to 15:1) to give the title compound as a yellow oil (300 mg, 87%).

WORKUP

后处理

  1. filtrationfiltered
  2. customto remove the solids
  3. customThe filtrate was evaporated in vacuo
  4. customthe crude residue obtained
  5. custompurified by column chromatography (petroleum ether:EtOAc, 100:1 to 15:1)