HRID2266589

反应详情

EQUATION

反应方程式

HRID 2266589 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of [3-(4-ethanesulfonylbenzyl)-8-fluoro-4-methyl-2-oxo-1,2-dihydroquinolin-5-yloxy]acetic acid methyl ester (0.33 g), N,N-dimethylformamide (5.0 mL), potassium carbonate (0.16 g) and acetic acid chlorodifluoromethyl ester (1.2 mL) was stirred at 70° C. for 3 days. The mixture was diluted with saturated aqueous ammonium chloride solution, extracted with ethyl acetate and the combined extracts washed with saturated aqueous sodium chloride solution and then dried over magnesium sulfate. The solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel, eluting with dichloromethane gave title as a white solid, 0.10 g.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washthe combined extracts washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure and purification of the residue by column chromatography on silica gel
  5. washeluting with dichloromethane
  6. customgave title as a white solid, 0.10 g