Reaktion #77590

ord-a55562a312b24b42ae7e2780f4d3957a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Einengenthe reaction mixture was concentrated under reduced pressure
  2. 2
    workup.ADDITIONEthanol (5.0 mL) was added to the residue
  3. 3
    Einengenthe mixture was concentrated under reduced pressure
  4. 4
    SonstigeThe residue was recrystallized from methanol-diethyl ether

Vorschrift

To a solution of N,N′-bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]-N,N′-dimethylethylenediamine (40.0 mg, 0.070 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.14 mL, 0.14 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 204.0-206.0° C.) (32.0 mg, yield: 60%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06706703B2uspto-grants-2004_03