HRID615660

反应详情

EQUATION

反应方程式

HRID 615660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of the 1,1-dimethylethyl ester product from part (a) (4.13 g., 7.73 mmole) and palladium hydroxide/carbon catalyst (400 mg.) in ethyl acetate (90 ml.) and ethanol (10 ml.) is stirred under a hydrogen atmosphere (balloon). The system is evacuated and refilled with fresh hydrogen every 30 minutes. After stirring for 3 hours, the catalyst is removed by filtration (Teflon millipore) and the filtrate is concentrated at reduced pressure to give 3.15 g. of 1-[N6 -](1,1-dimethylethoxy)carbonyl]-L-lysyl]-L-proline, 1,1-dimethylethyl ester as a colorless solid.

WORKUP

后处理

  1. customThe system is evacuated
  2. additionrefilled with fresh hydrogen every 30 minutes
  3. stirringAfter stirring for 3 hours
  4. customthe catalyst is removed by filtration (Teflon millipore) and the filtrate
  5. concentrationis concentrated at reduced pressure
  6. customto give 3.15 g