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ChemicalBook CAS DataBase List 2,4,6-Trichloropyridine
16063-69-7

2,4,6-Trichloropyridine synthesis

5synthesis methods
2,6-DICHLOROPYRIDINE N-OXIDE

2587-00-0

2,4,6-Trichloropyridine

16063-69-7

2,6-Dichloropyridine-N-oxide (Y-2) (8.20 g, 0.050 mol) was used as a raw material, which was dissolved in phosphorus trichloride (POCl3, 25 mL) and the reaction was carried out at reflux for 4 hours. After completion of the reaction, the solvent was removed by distillation under reduced pressure. The residue was carefully poured into crushed ice and extracted with petroleum ether (3 x 50 mL). The organic phases were combined, dried with anhydrous potassium carbonate (K2CO3), filtered and concentrated under reduced pressure. The crude product was purified by fast column chromatography using a mixed solvent of ethyl acetate/petroleum ether as eluent, resulting in colorless needle-like crystals of 2,4,6-trichloropyridine (Y-3) in 85% yield with a melting point of 32-33 °C. The final product was extracted from the crude product using a mixture of ethyl acetate/petroleum ether as eluent, and then dried with anhydrous potassium carbonate (3 × 50 mL).

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Yield:16063-69-7 85%

Reaction Conditions:

with trichlorophosphate for 4 h;Reflux;

Steps:

General procedure for synthesis of 2,4,6-trichloropyridine(Y-3)
General procedure for synthesis of 2,4,6-trichloropyridine(Y-3)
A mixture of 2,6-dichloropyridine-1-oxide (Y-2) (8.20 g, 0.050 mol) in POCl3 (25 mL) was refluxed for 4 h.
Then, the solvent was evaporated under reduced pressure.
The residue was poured into crushed ice and extracted with petroleum ether (3 * 50 mL).The combined organic phase was dried over K2CO3, filtered, and concentrated in vacuum.
The residue was further purified by flash column chromatography using ethyl acetate/petroleum ether as an eluent to give 2,4,6-trichloropyridine (Y-3) as colorless needles, yield 85%, mp: 32-33 °C.

References:

Yang, Jiapei;Chen, Wenmin;Kang, Dongwei;Lu, Xueyi;Li, Xiao;Liu, Zhaoqiang;Huang, Boshi;Daelemans, Dirk;Pannecouque, Christophe;De Clercq, Erik;Zhan, Peng;Liu, Xinyong [European Journal of Medicinal Chemistry,2016,vol. 109,p. 294 - 304]

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