Electric Literature of 246847-98-3, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 246847-98-3, name is 5-Chloro-3-fluoropyridin-2-amine. A new synthetic method of this compound is introduced below.
To concentrated sulfuric acid (100mL) cooled to -10 was added 2-amino-3-fluoro-5-chloropyridine (10 g, 68.2 mmol) with stirring. After dissolution, the mixture was continued to stir at -10 for 15min. Then 50 mL 30%hydrogen peroxide solution was added slowly, and the reaction temperature was maintained below 0. The mixture was warmed to room temperature and stirred for 72h, then poured into 500 mL 13%ice brine with stirring and extracetd with 200mL EA for three times. The combined organic extracts were washed with saturated sodium bicarbonate solution until the aqueous phase was alkaline, dried with anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography to give the desired product 2-nitro-3-fluoro-5-chloropyridine (2.8g, 23.3%) .
At the same time, in my other blogs, there are other synthetic methods of this type of compound,246847-98-3, 5-Chloro-3-fluoropyridin-2-amine, and friends who are interested can also refer to it.
Reference:
Patent; FUJIAN HAIXI PHARMACEUTICALS CO., LTD; FENG, Yan; WANG, Ruyong; LI, Junqing; ZHENG, Jianjia; LIAN, Xin; GONG, Xuan; FU, Yueli; KANG, Xinshan; (144 pag.)WO2019/174601; (2019); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem