HRID1088267

反应详情

EQUATION

反应方程式

HRID 1088267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(2S,4S)-1-(p-Nitrobenzyloxycarbonyl)-2-trichloroacetylaminocarbonyloxymethyl-4-acetylthiopyrrolidine (121 mg) was dissolved in 5.8 ml of methanol. To the solution was added 0.45 ml of 1N sodium hydroxide solution under ice-cooling in a nitrogen stream, followed by stirring at the same temperature for 40 minutes. After neutralization by 1.45 ml of 1N hydrochloric acid, the mixture was distilled to remove methanol. The residue was diluted with methylene chloride, washed with water, dried over anhydrous sodium sulfate and distilled to obtain (2S,4S)-1-(p-nitrobenzyloxycarbonyl)-2-aminocarbonyloxymethyl-4-mercaptopyrrolidine.

WORKUP

后处理

  1. temperaturecooling in a nitrogen stream
  2. distillationAfter neutralization by 1.45 ml of 1N hydrochloric acid, the mixture was distilled
  3. customto remove methanol
  4. additionThe residue was diluted with methylene chloride
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled