HRID248754

反应详情

EQUATION

反应方程式

HRID 248754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.79 g (40.57 mmol) of 2-[N-(4-fluoro-3-trifluoromethylphenyl)sulfamoyl]acetic acid methyl ester is dissolved in 110 ml of dioxane and combined with 59 ml (118 mmol) of 2N sodium hydroxide solution. The mixture heated up slightly, and the starting material had disappeared after 15 minutes. The mixture is concentrated to dryness under vacuum, the residue is combined with 2N hydrochloric acid, and the thus-precipitated acid is taken up in ethyl acetate. The organic solution is washed with water, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is crystallized from ethyl acetate/hexane. The title compound melts at 138°-140° C.

WORKUP

后处理

  1. temperatureThe mixture heated up slightly
  2. concentrationThe mixture is concentrated to dryness under vacuum
  3. washThe organic solution is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness under vacuum
  6. customThe residue is crystallized from ethyl acetate/hexane