HRID1088252

反应详情

EQUATION

反应方程式

HRID 1088252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trans-1-(p-Nitrobenzyloxycarbonyl)-4-benzoyloxy-L-proline p-methoxybenzyl ester (61.3 g) and anisole (12.8 ml) were stirred together with 70 ml of trifluoroacetic acid at room temperature for 30 minutes. The reaction mixture was distilled to remove tri-fluoroacetic acid, and the residue was diluted with ethyl acetate and a saturated sodium bicarbonate solution. The precipitated crystals were separated by filtration and dissolved in methanol. The solution was acidified with 6N hydrochloric acid to pH 1.0, diluted with ethyl acetate, washed with water and dried over anhydrous sodium sulfate. The solvent was removed by distillation to give trans-1-(p-nitrobenzyloxycarbonyl)-4-benzoyloxy-L-proline.

WORKUP

后处理

  1. distillationThe reaction mixture was distilled
  2. customto remove tri-fluoroacetic acid
  3. additionthe residue was diluted with ethyl acetate
  4. customThe precipitated crystals were separated by filtration
  5. dissolutiondissolved in methanol
  6. additiondiluted with ethyl acetate
  7. washwashed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. customThe solvent was removed by distillation