Methanesulfonic Acid → 1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]hexahydro-1,4-diazepine dimethanesulfonate

Participants

Reaction Steps

To a solution of 1,4-bis[5-(3,4,5-trimethoxylphenyl)-2-pyridyl]hexahydro-1,4-diazepine (72.4 g, 0.120 mol) in ethanol-chloroform (1:3, 600 mL) was added methanesulfonic acid (24.9 g, 0.258 mol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methanol-diethyl ether to yield the title compound as a slightly yellow crystalline powder (melting point: 204.0-206.0° C.) (88.2 g, yield: 92%).

Provenance & Evidence