HRID23954

反应详情

EQUATION

反应方程式

HRID 23954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

(R)-2-(4-methoxybenzoylamino)-2-phenylethyl azide (46.3 g) was combined with 10% palladium on carbon in THF (400 mL), methanol (100 mL) and was stirred under a hydrogen atmosphere. Analysis by TLC (70% methylene chloride, ethyl acetate) indicated absence of starting material after stirring overnight. The solution was filtered through diatomaceous earth, rinsed with THF, and evaporated. The resulting solid was recrystallized with ethyl acetate, and dried under vacuum at 60° C. for 1 h to afford 35.4 g (84%) of a white crystalline solid.

WORKUP

后处理

  1. stirringafter stirring overnight
  2. filtrationThe solution was filtered through diatomaceous earth
  3. washrinsed with THF
  4. customevaporated
  5. customThe resulting solid was recrystallized with ethyl acetate
  6. customdried under vacuum at 60° C. for 1 h