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ChemicalBook CAS DataBase List 2-Chloronicotinic acid
2942-59-8

2-Chloronicotinic acid synthesis

12synthesis methods
Chloronicotinic acid was synthesized from nicotinic acid by oxidation by H2O2 and then chlorinationby POCl3 and PCl5 in a yield of 87.5%.
Synthesis of 2-chloronicotinic acid: Pour chlorine gas into the mixed solution of phosphorus oxychloride and phosphorus trichloride, control the temperature at about 60°C, until the remaining chlorine gas escapes, cool and add nicotinic acid N-oxide in batches, and heat the mixed solution. The reaction was carried out at 100-105°C for 1-1.5 h, and the reaction mixture was stirred for 30 min after the reaction mixture was transparent, and phosphorus oxychloride was removed under reduced pressure. The obtained residue was cooled to room temperature, and water was added to obtain the finished product of 2-chloronicotinic acid.
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Yield:2942-59-8 98%

Reaction Conditions:

with sodium acetate;ozone;acetic acid at 20; for 5 h;Temperature;Reagent/catalyst;

Steps:

5

28.3 g (0.2 mol) of 2-chloro-3-ethylpyridine was added to a four-necked flask equipped with a mechanical stirrer and a thermometer, 100 mL of glacial acetic acid And sodium acetate0.82 g (0.01 mol). Room temperature stirring, the ozone generator oxygen 8.96L (0.4mol), 5h after the reaction solution in a large number of white solid production, TLC monitoring reaction processAfter the acetic acid decompression pumping system into the original volume of 1/3, filtered and dried white product 23.5g, yield 98%

References:

CN103848783,2016,B Location in patent:Paragraph 0029; 0030

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