HRID1417484

反应详情

EQUATION

反应方程式

HRID 1417484 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 ml of a 3% w/v aqueous solution of potassium hydroxide was added to a mixture of 44 mg of ethyl 2-(9-benzyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indol-2-yl)acetate (prepared as described in Example 82) in 2 ml of ethanol. The reaction mixture was then stirred at room temperature for 2 hours. At the end of this time, the reaction mixture was made acidic by the addition of a 3% w/v aqueous solution of hydrochloric acid and extracted with ethyl acetate. The ethyl acetate fraction was then washed with water and dried over anhydrous sodium sulfate. The solvent was then removed by evaporation under reduced pressure and the resulting residue was recrystallized from hexane and ethyl acetate to afford 37 mg of the title compound as a solid which melted at 164°-167° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate fraction was then washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was then removed by evaporation under reduced pressure
  5. customthe resulting residue was recrystallized from hexane and ethyl acetate