反应 #1885062

ord-ada1f94356914d2881663edc4805da97

反应方程式

NC[C@H](NC(=O)OCC1c2ccccc2-c2ccccc21)C(=O)C(=O)OCc1ccccc1
Fmoc-Dap-Z
CCNCC
diethylamine
NC[C@H](N)C(=O)C(=O)OCc1ccccc1
Dap-Z

试剂

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩the mixture is concentrated (bath temp. <30° C.)
  2. 2
    浓缩concentrated
  3. 3
    workup.ADDITIONTo the residue is added MeOH (20 mL) and CH2Cl2 (300 mL)
  4. 4
    浓缩the solution is concentrated
  5. 5
    浓缩toluene (400 mL), concentrated
  6. 6
    workup.WAITthe residue left under vacuum overnight
  7. 7
    其他to give product

实验过程

A 1-L round bottom flask is charged with Fmoc-Dap-Z, CH2Cl2 (122 mL) and diethylamine (61 mL, Acros). The solution is stirred at room temperature and the completion monitored by HPLC. After 7 hours, the mixture is concentrated (bath temp. <30° C.). The residue is suspended in CH2Cl2 (300 mL) and concentrated. This is repeated twice. To the residue is added MeOH (20 mL) and CH2Cl2 (300 mL), and the solution is concentrated. The residue is suspended in CH2Cl2 (100 mL) and toluene (400 mL), concentrated, and the residue left under vacuum overnight to give product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08343928B2uspto-grants-2013_01