HRID487526

反应详情

EQUATION

反应方程式

HRID 487526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethanol (3.6 g) and tetrahydrofuran (10 ml) were dropwise added to a solution of 2-chlorosulfonylbutyl chloride (14.4 g) and tetrahydrofuran (21 ml) while cooling with ice. After stirring at room temperature for 1 hour, ethyl p-aminobenzoylacetate (13.3 g), N,N-dimethylacetamide (33 ml) and pyridine (12.2 g) were added thereto, and the mixture was heated for refluxing for 30 minutes. 0.5 N hydrochloric acid (30 ml) was added to the reaction solution, and the mixture was extracted with ethyl acetate (120 ml). The extracted solution was washed with a sodium chloride aqueous solution (120 ml), then dried over magnesium sulfate, and concentrated. An oily product, ethyl p-(1-ethoxycarbonylpropanesulfonamido)benzoylacetate was quantitatively obtained.

WORKUP

后处理

  1. temperaturewhile cooling with ice
  2. temperaturethe mixture was heated
  3. temperaturefor refluxing for 30 minutes
  4. extractionthe mixture was extracted with ethyl acetate (120 ml)
  5. washThe extracted solution was washed with a sodium chloride aqueous solution (120 ml)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated