5-(Trifluoromethyl)-2-pyridinemethanamine synthesis
- Product Name:5-(Trifluoromethyl)-2-pyridinemethanamine
- CAS Number:164341-39-3
- Molecular formula:C7H7F3N2
- Molecular Weight:176.14
80194-70-3
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164341-39-3
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$55.00/100mg
Yield: 38%
Reaction Conditions:
with 5%-palladium/activated carbon;hydrogen in ethanol;water at 60; under 15001.5 - 18751.9 Torr; for 25 h;Autoclave;
Steps:
1 Comparative example 1
Into a 500mL autoclave, 20.85g (0.1mol, 99%, 1.0eq) of 2-cyano-3-chloro-5-trifluoromethylpyridine was sequentially added,5% palladium-carbon wet base 4.55g (54.5% water) and 170g ethanol.Replace the system with nitrogen three times and hydrogen three times,Pass hydrogen to the pressure in the kettle to 2.0-2.5Mpa,The temperature is controlled at 60 and the reaction is kept for about 20h without pressure lossContinue to incubate and react for 5 hours, take samples for HPLC control,The system is very complicated,The raw material remains about 5%, 2-aminomethyl-5-trifluoromethylpyridine is about 38%,One of the main impurities is about 40% of the product (secondary amine) obtained by removing one molecule of ammonia from two molecules of 2-aminomethyl-5-trifluoromethylpyridine.No post-processing was performed.
References:
Dalian Jiu Xin Fine Chemical Co., Ltd.;Wang Junchun;Wang Rongliang;Lv Chao;Wang Yanbo;Cong Xiaoqiang CN111170932, 2020, A Location in patent:Paragraph 0045-0046
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175277-74-4
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164341-39-3
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95727-86-9
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164341-39-3
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871826-12-9
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164341-39-3
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50488-42-1
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164341-39-3
93 suppliers
$55.00/100mg