HRID1820761

反应详情

EQUATION

反应方程式

HRID 1820761 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5 mmol of N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimid-hydrochloride was slowly added to a stirred suspension of 5 mmol 2-hydroxy-5-methanesulfonyl-benzoic acid, 5 mmol of benzyl alcohol and 0.5 mmol of 4-dimethylaminopyridine in 10 ml acetonitrile. The mixture was stirred overnight at room temperature, concentrated and treated with 10 ml of water. A few drops of diluted hydrochloric acid were added to acidify the solution. The resulting solid was filtered and then purified by chromatography (SiO2; ethyl acetate/cyclohexane 3:7) to yield the title compound as a colorless solid. MS (m/e): 305.0 (M−H, 100%)

WORKUP

后处理

  1. concentrationconcentrated
  2. additiontreated with 10 ml of water
  3. additionA few drops of diluted hydrochloric acid were added
  4. filtrationThe resulting solid was filtered
  5. custompurified by chromatography (SiO2; ethyl acetate/cyclohexane 3:7)