反応 #1904038

ord-b9190018bb9a41e0888f68096d43b3c7

反応方程式

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

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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