Reaktion #70482

ord-1f3c4c1675544c09b427902408c8625c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextract organics with EtOAc (3×50 mL)
  2. 2
    TrocknenCombined organic layers are dried over MgSO4
  3. 3
    Einengenconcentrated
  4. 4
    SonstigeResulting solid
  5. 5
    Sonstigeis triturated with EtOAc

Vorschrift

Combine 6-piperazin-1-yl-nicotinic acid ethyl ester (1.30 g, 5.40 mmol), 1,4-dichlorophthalazine (932 mg, 4.59 mmol), triethylamine (1.78 mL, 13.50 mmol), and NMP (8 mL) and heat to 85° C. for 6 h. Cool to room temperature, dilute with H2O (50 mL) and extract organics with EtOAc (3×50 mL). Combined organic layers are dried over MgSO4 and concentrated. Resulting solid is triturated with EtOAc to give the title compound as a fine tan powder (895 mg, 49% yield).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08536168B2uspto-grants-2013_09