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ChemicalBook CAS DataBase List 3-Amino-2-chloro-4-methylpyridine
133627-45-9

3-Amino-2-chloro-4-methylpyridine synthesis

11synthesis methods
3-Amino-2-chloro-4-methylpyridine can be obtained by reacting 2-chloro-4-methylnicotinamide with strong bases and halides.
3-Amino-2-chloro-4-methylpyridine
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Yield:133627-45-9 83.2%

Reaction Conditions:

Stage #1:3-amino-4-methylpyridine with hydrogenchloride in water at 40;Cooling with ice;
Stage #2: with dihydrogen peroxide for 2 h;

Steps:

4
First, 21.6 g of 3-amino-4-methylpyridine was added to the reaction kettle,In the cold water bath slowly dropping 72mL concentrated hydrochloric acid,Stirring to clarify after warming to 40 ° C, 30 ~ 60min slowly dropping 30mL 30% hydrogen peroxide, temperature control reaction 2h.After completion of the reaction, the system ρΗ = 3 was adjusted with 45% sodium hydroxide solution, extracted with trichloromethane, dried and removed to obtain the crude product. Recrystallization from petroleum ether or n-hexane gave white or pale yellow needle-like crystals of 2-chloro-3-amino-4-methylpyridine with a purity of 99.0%, a yield of 83.2%

References:

Hunan University;HU, AIXI;CHEN, AIYU;GU, YUPENG;NIE, JIANXIA;YE, JIAO CN106243022, 2016, A Location in patent:Paragraph 0076-0078

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