反応 #1885062

ord-ada1f94356914d2881663edc4805da97

反応方程式

試薬

なし

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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