3-Amino-2-chloro-4-methylpyridine synthesis
- Product Name:3-Amino-2-chloro-4-methylpyridine
- CAS Number:133627-45-9
- Molecular formula:C6H7ClN2
- Molecular Weight:142.59
3430-27-1
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133627-45-9
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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
152362-01-1
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133627-45-9
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23056-39-5
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133627-45-9
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5832-44-0
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65169-38-2
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133627-45-9
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