反应 #1904038

ord-b9190018bb9a41e0888f68096d43b3c7

反应方程式

N[C@@H](CC(=O)O)C(=O)O
aspartic acid
CCN(CC)CC
triethyl amine
O=C(Cl)CCC(=O)Cl
succinyl chloride
N[C@@H](CC(=O)O)C(=O)O.O=C1CCC(=O)N1
Aspartic Acid Succinimide

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他fitted with a condenser and nitrogen inlet
  2. 2
    温度refluxed for 6 hours
  3. 3
    过滤The triethyl amine hydrochloride is filtered
  4. 4
    浓缩the filtrate is concentrated
  5. 5
    其他by removing the solvent under vacuum
  6. 6
    其他The residue is used directly for the subsequent reaction
  7. 7
    其他The residue can be purified by chromatography on silica gel

实验过程

This example that demonstrates how this method could be performed. 9.4 g aspartic acid, 10 ml triethyl amine and 100 ml tetrahydrofuran are transferred into a 100 ml flask fitted with a condenser and nitrogen inlet. The mixture is cooled to 0° C. and 5 g succinyl chloride is added and the mixture stirred under nitrogen atmosphere for 5 min and refluxed for 6 hours. The triethyl amine hydrochloride is filtered and the filtrate is concentrated by removing the solvent under vacuum. The residue is used directly for the subsequent reaction. The residue can be purified by chromatography on silica gel.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07597882B2uspto-grants-2009_10