Reaktion #470730

ord-1288b427f58043569035589f0736fcc0

Lösungsmittel

Reaktionsbedingungen

Temperatur
130°CELSIUS
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
    Trocknen1:3, Ethyl Acetate:Petroleum ether, dried
  8. 8
    Filtrationover filter funnel in vacuo
  9. 9
    Sonstigeto yield a gray solid
  10. 10
    SonstigeA synthetic reaction scheme

Vorschrift

A mixture of 3-chloro-6-phenyl-4-(pyridin-4-yl)pyridazine (MW01-7-076WH) (0.5 mmol), 2-Morpholin-4-yl-ethylamine (2.0 mmol) in 3 ml of 1-BuOH was heated with stirring at 130° C. for about 7 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, then 1:3, Ethyl Acetate:Petroleum ether, dried over filter funnel in vacuo to yield a gray solid. ESI-MS: m/z 362.2 (M+H+). A synthetic reaction scheme for the preparation of 3-(4-methylpiperazin-1-yl)-N-(2-morpholinoethyl)-6-phenyl-4-(pyridin-4-yl)pyridazin-3-amine (MW01-7-091WH) is depicted in FIG. 10.

Quelle

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