HRID18037

反应详情

EQUATION

反应方程式

HRID 18037 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

635.62 mg of N,N′-carbonyldiimidazole are added to a solution of 200 mg of the compound of Example 3 in 90 ml of 2-butanone. The reaction mixture is refluxed for 4 days under argon and then, after cooling, diluted with an aqueous 5% Na2CO3 solution (15 ml) and extracted with ethyl acetate. The organic solutions are combined, dried over anhydrous sodium sulphate, filtered and then evaporated to dryness under reduced pressure. Chromatography on silica gel (dichloromethane and then a gradient of methanol in dichloromethane of from 0.1 to 1.5%) allow 78 mg of the expected product to be isolated.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 4 days under argon
  2. temperatureafter cooling
  3. extractionextracted with ethyl acetate
  4. dry with materialdried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. customevaporated to dryness under reduced pressure
  7. customto be isolated