Reaktion #68776

ord-35c558e166d3439c925f4ad65b21b742

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirring
  2. 2
    workup.WAITis continued over night
  3. 3
    workup.ADDITIONThe mixture is poured on water
  4. 4
    Extraktionis extracted with ethyl acetate
  5. 5
    TrocknenThe combined organic layers are dried over sodium sulphate
  6. 6
    Sonstigethe solvent is removed in vacuo
  7. 7
    SonstigeThe residue is triturated with DCM

Vorschrift

To 5.0 g (44.6 mmol) 4-pyrazolecarboxylic acid in 100 mL DMF 15.2 mL (89.2 mmol) DIPEA and 15.7 g (49.1 mmol) TBTU are added and the mixture is stirred for 10 min at rt. Subsequently 8.9 g (44.6 mmol) (S)-1-(4-bromophenyl)ethylamine are added and stirring is continued over night. The mixture is poured on water and is extracted with ethyl acetate. The combined organic layers are dried over sodium sulphate and the solvent is removed in vacuo. The residue is triturated with DCM to yield the desired product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530461B2uspto-grants-2013_09