反応 #77589

反応方程式

1,4-bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]piperazine

methanesulfonic acid

methanol

→

title compound

収率 82.0%

1,4-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]piperazine Dimethanesulfonate

収率 82.0%

溶媒

methylene chloride

反応条件

後処理

1. 1
   濃縮the reaction mixture was concentrated under reduced pressure
2. 2
   その他The residue was recrystallized from methylene chloride-diethyl ether

実験手順

To a solution of 1,4-bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]piperazine (147.0 mg, 0.257 mmol) in methylene chloride (5.0 mL) was added a 1.0 M solution of methanesulfonic acid in methanol (0.54 mL, 0.54 mmol), and the reaction mixture was concentrated under reduced pressure. The residue was recrystallized from methylene chloride-diethyl ether to yield the title compound as a pale yellow crystalline powder (melting point: 238.0-239.0° C.) (160.8 mg, yield: 82%).

出典