반응 #77590

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N,N′-bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]-N,N′-dimethylethylenediamine

methanesulfonic acid

→

title compound

수율 60.0%

N,N′-Bis[5-(3,4,5-trimethoxyphenyl)-2-pyridyl]-N,N′-dimethylethylenediamine Dimethanesulfonate

수율 60.0%

용매

methanol

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후처리

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

실험 절차

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%).

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