Preparation method and use of 2-amino-4-chloro-pyridine
2-Amino-4-chloro-pyridine is a white solid. 4-Chloropyridine-2-amide can be prepared from 2-pyridine carboxylic acid as raw material, and then reacted with calcium hypochlorite to obtain 2-amino-4-chloropyridine-Pyridine. 2-Amino-4-chloro-pyridine can be used to prepare 4-fluoro-2-aminopyridine, 4-fluoro-2-aminopyridine is used for the preparation of tyrosine kinase inhibitors, P13K inhibitors, and aldosterone synthase inhibitors. It is an important intermediate of inhibitors and has broad application prospects.

2-amino-4-chloro-pyridine

Preparation method of 2-amino-4-chloro-pyridine
40 grams of 2-pyridine carboxylic acid was slowly added to 116 grams of thionyl chloride, and after the addition, 1 gram of N, N-dimethylformamide was added, and the reaction solution was refluxed for 2-16 hours until the reaction of the raw materials was completed. The thionyl chloride was recovered to obtain 46 g of 4-chloropyridine-2-acid chloride; 4-chloropyridine-2-acid chloride was dissolved in 200 ml of 1,4-dioxane, and ammonia gas was passed into it for 5-16 hours After the reaction was completed, most of the solvent was removed, the temperature was lowered to 0-5° C., and a white solid was precipitated and dried to obtain 4-chloropyridine-2-amide, 37 g, yield 93%.

35 grams of 4-chloropyridine-2-amide were added to the calcium hypochlorite aqueous solution in batches, and the calcium hypochlorite aqueous solution was prepared from 78 grams of calcium hypochlorite and 1 liter of water, and the addition was heated to 60-80 ° C for reaction After the raw materials were consumed, the temperature was cooled to room temperature, the reaction solution was extracted with dichloromethane until there was no product in the aqueous phase, the organic phase was dried over anhydrous sodium sulfate, the solvent was removed, and the white solid was recrystallized from ethanol, 30 g, yield 81%.

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