Reaktion #161686

ord-9cfe5f1b925142c4b3372c5a4f8eccb9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGstirred for 10 min
  2. 2
    workup.STIRRINGAfter vigorous stirring the solid
  3. 3
    Filtrationfiltered
  4. 4
    Sonstigedried in the CAD

Vorschrift

2.80 g (10.2 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 6.00 mL (34.9 mmol) DIPEA were added to 1.90 g (10.2 mmol) ethyl 6-chloropyrimidine-4-carboxylate in 60 mL DMF and the reaction mixture was stirred for 3 h at RT. After elimination of the solvent i. vac. the residue was combined with 70 mL water and stirred for 10 min. 5 mL ethyl acetate were added. After vigorous stirring the solid was suction filtered and dried in the CAD.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829006B2uspto-grants-2014_09