Reaktion #470735
ord-32675221a6a947b8860894d33ee80b2a
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturwas heated
- 2SonstigeThe solvent was removed by evaporation in vacuo
- 3workup.ADDITIONthe residue was treated with water
- 4Sonstigeto give a suspension
- 5FiltrationThe solid was then filtered off
- 6Waschenwashed with water
- 7Sonstigedried
- 8Filtrationover filter funnel in vacuo
- 9Sonstigeto 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).