HRID840588

反应详情

EQUATION

反应方程式

HRID 840588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 4-nitrobenzylamine hydrochloride (10.3 g, 54.7 mmol) and triethylamine (11.1 g, 109 mmol) in dichloromethane (75 mL) was added a solution of di-tert-butyldicarbonate (15.5 g, 71.1 mmol) in dichloromethane (25 L). After stirring overnight at room temperature, the reaction was washed with 10k citric acid (2×250 mL), dried over magnesium sulfate, filtered, and the solvent removed under reduced pressure. The residue was recrystallized from ethyl acetate/hexanes to afford the 13.80 g of the title compound. (100%).

WORKUP

后处理

  1. washthe reaction was washed with 10k citric acid (2×250 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. customthe solvent removed under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate/hexanes