HRID2251251

反应详情

EQUATION

反应方程式

HRID 2251251 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To 2.47 mol sodium sulfite in 1120 ml water at RT was added dropwise over 20 min a solution of 329 mmol 3,4-difluoro-benzenesulfonyl chloride in 560 ml dioxane and stirring continued for a further 30 min. 1 M aq NaOH was then added dropwise until the reaction mixture was pH 14, and the mixture was then allowed to stir at RT for a further 16 h. The mixture was then cooled to 0° C. and concentrated H2SO4 added until the reaction mixture was pH 1. The mixture was extracted three times with ethyl acetate, and the combined organic phases washed with saturated aq NaCl solution and then dried with Na2SO4. Evaporation in vacuo yielded the title compound. MS (m/e): 177.1 ([M−H]−, 100%)

WORKUP

后处理

  1. stirringto stir at RT for a further 16 h
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washthe combined organic phases washed with saturated aq NaCl solution
  4. dry with materialdried with Na2SO4
  5. customEvaporation in vacuo