Reaktion #470735

ord-32675221a6a947b8860894d33ee80b2a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    SonstigeThe solvent was removed by evaporation in vacuo
  3. 3
    workup.ADDITIONthe residue was treated with water
  4. 4
    Sonstigeto give a suspension
  5. 5
    FiltrationThe solid was then filtered off
  6. 6
    Waschenwashed with water
  7. 7
    Sonstigedried
  8. 8
    Filtrationover filter funnel in vacuo
  9. 9
    Sonstigeto give light pink solid

Vorschrift

A mixture of 3-chloro-4,6-diphenylpyridazine (267 mg, 11.0 mmol), 1-(2-pyrimidyl)piperazine (656 mg, 4.0 mmol) in 3 ml of 1-BuOH was heated with stirring at 130 C for 3 days. The solvent was removed by evaporation in vacuo, the residue was treated with water to give a suspension. The solid was then filtered off, washed with water, dried over filter funnel in vacuo to give light pink solid. (320 mg, 0.81 mmol, yield 81.1%). ESI-MS: m/z 395.5 (M+H+). HRMS calcd 395.1979. found 395.1973. 1H NMR (CDCl3): d 8.329 (d, J=5.0, 2H), 8.101 (d, J=7.5, 2H), 7.734 (d, J=7.5, 2H), 7.655 (s, 1H), 7.509 (m, 6H), 6.530 (t, J=4.5, 1H), 3.836 (t, J=4.5, J=5.0, 4H), 3.394 (t, J=5.0, J=4.5, 4H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08367672B2uspto-grants-2013_02