Reaction #1885062

ord-ada1f94356914d2881663edc4805da97

Reaction equation

Reagents

None

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

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

Procedure

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08343928B2uspto-grants-2013_01