Electric Literature of 13466-35-8 , The common heterocyclic compound, 13466-35-8, name is 3-Chloro-2-hydroxypyridine, molecular formula is C5H4ClNO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
To a 500 ml four-necked flask equipped with a thermometer, mechanical stirring, and a reflux condenser was added 150 g of 1,2-dichloroethane, 26.0 g (0.2 mol) of 2-hydroxy-3-chloropyridine prepared in Example 3, 52.0 g (0.25 mole) of phosphorus pentachloride, stir the reaction at 60-65 C for 10 hours, then slowly pour the residue into 200 g of ice water, stir well, and then neutralize the pH value with a 40 wt% sodium hydroxide aqueous solution. 8. The layers were separated. The aqueous layer was 50g with 1,2-dichloroethane three times. The organic phases were combined, washed with 30g of saturated brine, and then dried with 5g of anhydrous sodium sulfate. The solvent was removed by rotary evaporation. 28.1 g of 2,3-dichloropyridine (I) with a yield of 94.9% and a gas phase purity of 99.9%.
The synthetic route of 13466-35-8 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Sun Yulong; Zhang Mingfeng; Chang Renyi; Wang Tao; (10 pag.)CN110818622; (2020); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem