HRID976020

反应详情

EQUATION

反应方程式

HRID 976020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Meso-2,3-bis(benzylamino)succinic acid (9.5 g, 0.029 mol) was dissolved in a mixture of glacial acetic acid (50 ml) and concentrated hydrochloric acid (50 ml). Hydrogenolysis was effected at ambient temperature with 10% palladium on charcoal (1.0 g) as catalyst. The reaction was run until NMR showed that unreacted starting material was no longer present. Water (100 ml) was added and the catalyst was removed by filtration. The filtrate was concentrated (rotavapor) and the residue was dissolved in dilute aqueous sodium hydroxide. pH was adjusted to approximately 5 upon addition of glacial acetic acid. Crystals were filtered off and washed.

WORKUP

后处理

  1. customthe catalyst was removed by filtration
  2. concentrationThe filtrate was concentrated (rotavapor)
  3. dissolutionthe residue was dissolved in dilute aqueous sodium hydroxide
  4. additionpH was adjusted to approximately 5 upon addition of glacial acetic acid
  5. filtrationCrystals were filtered off
  6. washwashed