Reaktion #161685

ord-bbc93f1415f8483fa6db930c91c452c8

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISSOLUTIONhad dissolved
  2. 2
    Filtrationfiltered
  3. 3
    Sonstigedried at 50° C. in the CAD

Vorschrift

590 mg (1.49 mmol) ethyl 6-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylate, 20 mL ethanol, 1 mL water and 1 mL (4.0 mmol) of a 4M NaOH solution were stirred for 2 h at RT. The reaction mixture was diluted with water until the precipitate had dissolved. 1 mL of a 4M hydrochloric acid solution were added and the ethanol was eliminated i. vac. The reaction mixture was stirred for 30 min at RT, the precipitate was suction filtered and dried at 50° C. in the CAD.

Quelle

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