4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline
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4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline
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CAS No:
694499-26-8
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Formula:
C13H18F3N3
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Chemical Name:
4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline
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Synonyms:
4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)a
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CAS No:
4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline Basic Attributes
273.3
273.145294
2933599090
4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline Use and Manufacturing
400mL THF was added to a 2L reaction kettle, cooled to -5 ° C or less, was added portionwise aluminum hydrideLithium 50g (l. 33mol, 4. Oeq), stirred lOmin, continue to -5 ° C or less, and began dropping aluminum trichloride10g (0. 0667mol, 0. 2eq) in THF solution. Keeping the temperature below 5 ° C, then stirred for 30min after beginning coupled step dropsThe product amide 96g (0. 334mol, 1. Oeq) was dissolved in 500mL THF solution, the temperature is still below 5 ° C, after increases room temperatureStirring. Disappearance of starting materials monitored by TLC the reaction was complete. Cooled to 0 ° C or less, and began dropping water to quench the reaction. Filtered and the filtrateRotary done crude was crystallized from toluene once in pure 60. 5g, Yield: 60percentTo a solution of vitride (3 equiv) in toluene (6times) under nitrogen atmosphere was slowly added lot wise [4-amino-2-(trifluoromethyl) phenyl] -(4-methylpiperazin-l- yl)methanone (1 equiv) at room temperature during 2h (exothermic). After stirring for 4h at 65°C, slowly added 8percent aq. NaOH solution (12 equiv) during lh at room temperature. Resulting solution was stirred for 30minutes, extracted with toluene, combined toluene layers were dried over Na
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4-(4-Methylpiperazinomethyl)-3-(trifluoromethyl)aniline
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