反应 #1904036

ord-cb3eda1f623b4d299c253947c39dfc07

反应方程式

NCCCC[C@H](N)C(=O)O
Lysine
O=C1CCCC(=O)O1
glutaric anhydride
CN(C)C=O
DMF
NC(=O)CCCC(N)=O.NCCCC[C@H](N)C(=O)O
Lysine Glutaramide

反应条件

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
    其他immersed into an oil bath
  3. 3
    workup.WAITpreheated to 90° C. for 1.5 h until HPLC assay
  4. 4
    其他completion of reaction
  5. 5
    其他DMF is evaporated under vacuum (
  6. 6
    workup.DISTILLATIONdistilled below 40° C.
  7. 7
    其他the residue is used directly for the subsequent reaction
  8. 8
    其他The residue can be purified by chromatography on silica gel

实验过程

In this example that demonstrates how this method could be performed, 5 g Lysine, 8.7 g glutaric anhydride and 2.0 g 4-Dimethylaminopyridine (DMAP) are weighed into a 100 ml flask fitted with a condenser and nitrogen inlet. 100 ml DMF is added and the mixture stirred under nitrogen atmosphere for 5 min and immersed into an oil bath preheated to 90° C. for 1.5 h until HPLC assay indicated completion of reaction. DMF is evaporated under vacuum (distilled below 40° C. and 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