Reaktion #77581

Reaktionsgleichung

1,4-bis[5-(3-hydroxy-4,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine

methanesulfonic acid

→

title compound

Ausbeute 65.8%

1,4-Bis[5-(3-hydroxy-4,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine Dimethanesulfonate

Ausbeute 65.8%

Lösungsmittel

methanol

Reaktionsbedingungen

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 resulting mixture was concentrated under reduced pressure
4. 4
   SonstigeThe residue was recrystallized from methanol

Vorschrift

To a solution of 1,4-bis[5-(3-hydroxy-4,5-dimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine (97.0 mg, 0.170 mmol) in methanol (5.0 mL) was added a 1.0 M aqueous methanesulfonic acid (0.35 mL, 0.35 mmol), and the reaction mixture was concentrated under reduced pressure. Ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from methanol to yield the title compound as a colorless crystalline powder (melting point: 300.0-301.0° C.) (84.0 mg, yield: 63%).

Quelle