2,4,6-Trichloropyridine synthesis
- Product Name:2,4,6-Trichloropyridine
- CAS Number:16063-69-7
- Molecular formula:C5H2Cl3N
- Molecular Weight:182.44
2587-00-0
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).
2587-00-0
200 suppliers
$20.00/1g
16063-69-7
224 suppliers
$40.00/5g
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]
2587-02-2
322 suppliers
$12.40/250mg
16063-69-7
224 suppliers
$40.00/5g
98027-84-0
210 suppliers
$6.00/1g
16063-69-7
224 suppliers
$40.00/5g
2402-78-0
518 suppliers
$6.00/25g
16063-69-7
224 suppliers
$40.00/5g
116632-24-7
170 suppliers
$10.00/250mg
16063-69-7
224 suppliers
$40.00/5g