HRID53334

反应详情

EQUATION

反应方程式

HRID 53334 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-[2-[(4-chlorophenyl)sulphonylamino]ethyl]-5-(4-fluorobenzoyl)benzenepropanoic acid (0.25 g) and potassium carbonate (0.212 g) in anhydrous methanol (5.0 ml) was heated under reflux for 18 hours. Additional potassium carbonate (0.212 g) was added and the mixture was heated under reflux for a further 20 hours and then cooled. Water (15 ml) was added and the solution was evaporated to about 10 ml and then acidified with 2N hydrochloric acid. The mixture was extracted several times with ethyl acetate and the combined extracts were washed with water and dried (MgSO4). Evaporation of the solvent gave the title compound as a glass (0.22 g). Found: C,60.25; H,4.92; N,2.51. C25H24ClNO6S requires C,59.81; H,4.82; N,2.79%.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for a further 20 hours
  5. temperaturecooled
  6. customthe solution was evaporated to about 10 ml
  7. extractionThe mixture was extracted several times with ethyl acetate
  8. washthe combined extracts were washed with water
  9. dry with materialdried (MgSO4)
  10. customEvaporation of the solvent