2-Amino-5-chloro-3-fluoropyridine synthesis
- Product Name:2-Amino-5-chloro-3-fluoropyridine
- CAS Number:246847-98-3
- Molecular formula:C5H4ClFN2
- Molecular Weight:146.55
89402-43-7
246847-98-3
General procedure for the synthesis of 2-amino-3-fluoro-5-chloropyridine from 2,3-difluoro-5-chloropyridine: 5-chloro-2,3-difluoropyridine (100 g, 0.669 mol) and liquid ammonia (1.125 L, 8.025 mol) were placed in an autoclave. The kettle was sealed and the reaction was carried out at 120 °C for 24 hours. Upon completion of the reaction, the reaction mixture was cooled and formation of a yellowish solid precipitate was observed. The precipitate was separated by filtration and the filter cake was washed with deionized water. The filtrate was extracted with ethyl acetate, the organic layers were combined and dried with anhydrous sodium sulfate. Subsequently, the organic solvent was removed by distillation under reduced pressure, and a small amount of petroleum ether was added to the residue, which was filtered again to obtain a precipitate of the target compound 2-amino-3-fluoro-5-chloropyridine. The final product was obtained as 84.22 g in 85.94% yield.
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Yield: 85.94%
Reaction Conditions:
with ammonia at 120; for 24 h;Autoclave;Temperature;
Steps:
6.A A.2-amino-3-fluoro-5-chloropyridine
5-chloro-2,3-difluoro-pyridine (100g, 0.669mol) and ammonia (1.125L, 8.025mol) added to the autoclave.After the reaction 120 sealed 24h, the reaction was complete, the cooling pale yellow solid precipitation, filtration, the filter cake was washed with water, and the filtrate was extracted with ethyl acetate, and the combined organic layer was dried over anhydrous sodium sulfate, the organic phase was distilled off under reduced pressure, with beating a small amount of petroleum ether, filtration, and precipitation cake cake obtained will be collected at the same time to give the compound 2-amino-3-fluoro-5-chloropyridine 84.22g, yield 85.94%.
References:
Guizhou University;Zhao, Chunshen;Chai, Huifang;Liu, LI;Huang, Zhuyan;Le, Yi CN105669539, 2016, A Location in patent:Paragraph 0058; 0059; 0060
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246847-98-3
121 suppliers
$6.00/1g