HRID1596690

反应详情

EQUATION

反应方程式

HRID 1596690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 25.0 g (74.1 mmol) (S)-2-(benzyloxycarbonylamino)pentanedioic acid 1-tert.-butyl ester (prepared according to Liebigs Ann. Chem. 1961, 646, 127) in 500 ml dry methanol were added 2.5 g 10% Pd/C, and the mixture was stirred over night at room temperature under an atmosphere of hydrogen. The catalyst was removed by filtration through celite and the filtrate was concentrated under reduced pressure. The remaining solid title compound was purified by stirring with a small amount of ethanol, filtered with suction, and dried in vacuo. Another crop (1.7 g) was obtained after concentration of the mother liquid and stirring of the residue with ethyl acetate.

WORKUP

后处理

  1. customThe catalyst was removed by filtration through celite
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe remaining solid title compound was purified
  4. stirringby stirring with a small amount of ethanol
  5. filtrationfiltered with suction
  6. customdried in vacuo
  7. customAnother crop (1.7 g) was obtained after concentration of the mother liquid