Reaktion #2452118

ord-c7059a9b925344ac8b10595ff68b7bbf

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe obtained urea was filtrated
  2. 2
    Sonstigethe solution was evaporated
  3. 3
    workup.DISSOLUTIONThe residue, dissolved in 10 ml acetonitrile
  4. 4
    workup.ADDITIONwas added
  5. 5
    SonstigeThe solvent was evaporated under vacuum
  6. 6
    Sonstigethe product was recrystallized from acetonitrile or acetone

Vorschrift

6.55 g (50 mMol) 3-dimethylamino-butyric acid 20 was added to 5.75 g (50 mMol) N-hydroxysuccinimide and 11.05 g (55 mMol) dicyclohexyl carbodiimide in 100 ml CH2Cl2. The reaction mixture was stirred for 16 h at RT. The obtained urea was filtrated and the solution was evaporated. The residue, dissolved in 10 ml acetonitrile, was added under stirring to a solution of 9.51 g (50 mMol) 4-toluenesulfonic acid monohydrate in acetonitrile (30 ml). The solvent was evaporated under vacuum and the product was recrystallized from acetonitrile or acetone.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08697604B2uspto-grants-2014_04