Реакция #1904038

ord-b9190018bb9a41e0888f68096d43b3c7

Уравнение реакции

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

Реагенты

Нет

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеfitted with a condenser and nitrogen inlet
  2. 2
    Температураrefluxed for 6 hours
  3. 3
    ФильтрацияThe triethyl amine hydrochloride is filtered
  4. 4
    Концентрированиеthe filtrate is concentrated
  5. 5
    Другоеby removing the solvent under vacuum
  6. 6
    ДругоеThe residue is used directly for the subsequent reaction
  7. 7
    ДругоеThe residue can be purified by chromatography on silica gel

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07597882B2uspto-grants-2009_10