HRID400991

反应详情

EQUATION

反应方程式

HRID 400991 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

360.0 g of the starting material, N-Boc-Asp(O-t-Bu)OH, together with Boc2O (353.0 g) and ammonium bicarbonate (NH4HCO3, 123.9 g) was added to dimethylformamide (1174.6 g), and pyridine (61.0 g) was added dropwise thereto at room temperature, and the reaction mixture was then stirred for about 3 hours. Upon completion of the reaction, water (1440 ml) and toluene (1800 ml) were added to the reaction solution and stirred for 30 minutes to separate the layers. The organic layer thus obtained was distilled under reduced pressure to remove t-butanol and toluene to obtain the title compound, which was directly used in the next reaction.

WORKUP

后处理

  1. additionwas added dropwise
  2. additionwere added to the reaction solution
  3. stirringstirred for 30 minutes
  4. customto separate the layers
  5. customThe organic layer thus obtained
  6. distillationwas distilled under reduced pressure
  7. customto remove t-butanol and toluene