HRID10421

反应详情

EQUATION

反应方程式

HRID 10421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.6 g of di-tert-butyl (2S,5S)-5-(2-benzylamino-2-cyanoethyl)pyrrolidine-1,2-dicarboxylate were dissolved in 6.5 ml of dimethyl sulfoxide. 373 mg of finely ground potassium carbonate and 1.08 ml of a 30% strength hydrogen peroxide solution were added thereto. The mixture was stirred at room temperature for 14 h and was then heated at 35° C. for 30 min. The solution was diluted with 60 ml of water and extracted 3 times with 100 ml of ethyl acetate each time. The combined organic phases were washed once with 120 ml of a saturated sodium chloride solution and dried with sodium sulfate. The solvents were removed in vacuo, and the residue was chromatographed on silica gel.

WORKUP

后处理

  1. temperaturewas then heated at 35° C. for 30 min
  2. extractionextracted 3 times with 100 ml of ethyl acetate each time
  3. washThe combined organic phases were washed once with 120 ml of a saturated sodium chloride solution
  4. dry with materialdried with sodium sulfate
  5. customThe solvents were removed in vacuo
  6. customthe residue was chromatographed on silica gel