Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 152460-09-8, name is N-(2-Methyl-5-nitrophenyl)-4-(pyridin-3-yl)pyrimidin-2-amine. A new synthetic method of this compound is introduced below., Quality Control of N-(2-Methyl-5-nitrophenyl)-4-(pyridin-3-yl)pyrimidin-2-amine
170 L of Cone. Hydrochloric acid is charged into the reactor. 70 Kg of stannous chloride dihydrate is charged. Stirred for 10 minutes. Cooled the reaction mass to 0-5C. Added compound of the formula (VI) slowly during 3-4 hours at 0-5 C. reaction mass is brought to 25-35C. Maintained 1 V2 hour at 25-35C. Charged 500 Its of DM water to the reaction mass and charged slowly 400 L of 50% sodium hydroxide solution at 25-3 5C. Reaction mass is extracted with 2 x 250 L chloroform. The chloroform layer is water wash thoroughly and carbon treatment is given . Distilled off chloroform completely under vacuum and charged 20 L ethyl acetate. Cooled to 0-10C. Maintained 1 hour at 0-10C. Centrifuged and washed with 10 L ethyl acetate to provide N-(5-amino-2-methyl phenyl)-4-(3-pyridyl)-2-pyrimidineamine of the formula [VII]Yield: 10 Kg (61.5%)MR: 141-144C.PuritybyHPLC:99.8%.Step -3:The preparation of N-(5-amino-2-methyl phenyl)-4-(3-pyridyl)-2-pyrimidineamine (VII)20 L of Cone. Hydrochloric acid is charged into the reactor. 7 Kg of stannous chloridedihydrate is charged. Stirred for 10 minutes. Cooled the reaction mass to 0-5C. Addedcompound of the formula (VI) slowly during 2-3 hours at 0-5C. reaction mass is broughtto 25-35C. Maintained 3 hours at 25-35C. Charged 500 Its of DM water to thereaction mass and charged slowly 40 L of 50% sodium hydroxide solution at 25-35C.Reaction mass is extracted with 2 x 35 L chloroform. The chloroform layer is waterwash thoroughly and carbon treatment is given . Distilled off chloroform completelyunder vacuum and charged 2 L ethyl acetate. Cooled to 0-10C. Maintained 1 hour at 0-10C. Centrifuged and washed with 1 L ethyl acetate to provide N-(5-amino-2-methylphenyi)-4-(3-pyridyl)-2-pyrimidineamine of the formula [VII]Yield: 0.98Kg(60%)MR: 140-143C.Purity by HPLC: 99.8%.Step -3: The preparation of N-(5-amino-2-methyl phenyl)-4-(3-pyridyl)-2-pyrimidineamine of theformula [VH] 17 L of Cone. Hydrochloric acid is charged into the reactor. 7 Kg of stannous chloride dihydrate is charged. Stirred for 10 minutes. Cooled the reaction mass to 0-5C. Added compound of the formula (VI) slowly during 2-3 hours at 0-5C. reaction mass is brought to 25-35C. Maintained 3 hours at 25-35C. Charged 500 Its of DM water to the reaction mass and charged slowly 40 L of 50% sodium hydroxide solution at 25-35C. Reaction mass is extracted with 2 x 50 L chloroform. The chloroform layer is waterwash thoroughly and carbon treatment is given . Distilled off chloroform completelyunder vacuum and charged 2 L ethyl acetate. Cooled to 0-10C. Maintainedl hour at 0-10C. Centrifuged and washed with 1 L ethyl acetate to provide N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidineamine of the formula [VII]Yield : 0.97 Kg (60%)MR: 140-143C.Purity by HPLC: 99.7%. Step -3 ;The preparation of N-(5-amino-2-methyl phenyl)-4-(3-pyridyl)-2-pyrimidineamine of theformula [VII]19 L of Cone. Hydrochloric acid is charged into the reactor. 7 Kg of stannous chloridedihydrate is charged. Stirred for 10 minutes. Cooled the reaction mass to 0-5C. Addedcompound of the formula (VI) slowly during 2-3 hours at 0-5C. reaction mass is broughtto 25-35C. Maintained 2 1A hour at 25-35C. Charged 500 Its of DM water to thereaction mass and charged slowly 40 L of 50% sodium hydroxide solution at 25-35C.Reaction mass is extracted with 2 x 50 L chloroform. The chloroform layer is waterwash thoroughly and carbon treatment is given . Distilled off chloroform completelyunder vacuum and charged 2 L ethyl acetate. Cooled to 0-10C. Maintained 1 hour at 0-10C. Centrifuged and washed with 1 L ethyl acetate to provide N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-pyrimidineamine of the formula [VII]Yield: 1.05 Kg (64.5%)MR: 142-144C.Purity by HPLC: 99.85%.
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Reference:
Patent; NATCO PHARMA LIMITED; KOMPELLA, Amala; BHUJANGA RAO, Adibhatla, Kali, Sathya; VENKAIAH CHOWDARY, Nannapaneni; WO2004/108699; (2004); A1;,
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