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Synthesis method of pyrazine-2, 3-dicarboxylic acid bis [(5-chloro-pyridine-2-yl)-amide]
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A synthesis method, technology of dicarboxylic acid, applied in the direction of organic chemistry etc.
Pending Publication Date: 2022-06-14
JIANGSU TASLY DIYI PHARMA CO LTD
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[0011] At present, there is no relevant report on this impurity in the domestic literature. The control of drugimpurity profile is an important measure to ensure the safety and effectiveness of drugs, and it is also a key link to improve the quality of domestic drugs. In order to facilitate the process research and quality control of zopiclone Purity impurity reference substance, urgently need to provide a kind of easy, low-cost method for preparing this impurity
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Embodiment 1
[0045] Embodiment 1: a kind of synthetic method of pyrazine-2,3-dicarboxylic acid bis[(5-chloro-pyridin-2-yl)-amide]
[0046] 3-(5-Chloropyridine-2-carbamoyl)-2-pyrazinecarboxylic acid (G) (5.57 g, 20 mmol), triethylamine (4.04 g, 40 mmol), EDCI (4.60 g, 24 mmol), HOBt (3.24 g, 24 mmol) was dispersed in dichloromethane (50 ml, 8.98 times the volume of the weight of compound G), and stirred for 10 minutes. 2-Amino-5-chloropyridine (2.57 g, 20 mmol) was added to the reaction mixture, and the reaction was refluxed for 16 hours.
[0050] Embodiment 2: A kind of synthetic method of pyrazine-2,3-dicarboxylic acid bis[(5-chloro-pyridin-2-yl)-amide]
[0051] 3-(5-Chloropyridine-2-carbamoyl)-2-pyrazinecarboxylic acid (Compound G) (5.57 g, 20 mmol), triethylamine (4.04 g, 40 mmol), EDCI (4.60 g, 24 mmol), HOBt (3.24 g, 24 mmol) was dispersed in DMF (50 ml, 8.98 times the volume of the weight of compound G) and stirred for 10 minutes. 2-Amino-5-chloropyridine (2.57 g, 20 mmol) was added to the reaction mixture, and the reaction was carried out at 100° C. for 16 hours.
[0052] The reaction mixture was gradually cooled to room temperature, water was added and stirred, then 50 mL of dichloromethane was added to the aqueous phase for extraction twice, the organic phases were combined, the aqueous phase was extracted twice with dichloromethane, the organic phases were combined and washed once with saturated brine, Dry over magnesiumsulfate and filter. After the filtrate was concentrated, column chromatography (...
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Abstract
The invention relates to a synthesis method of pyrazine-2, 3-dicarboxylic acid bis [(5-chloro-pyridine-2-yl)-amide], which comprises the following steps: 1) by taking 3-(5-chloropyridine-2-carbamyl)-2-pyrazinecarboxylic acid (compound G) as a raw material, adding triethylamine, EDCI, HOBt and 2-amino-5-chloropyridine into an organic solvent for condensation reaction, and stirring for 4-18 hours; (2) after the reaction is finished, pouring reaction liquid into water, extracting and separating; and (3) purifying the isolate through a purification column to obtain a pyrazine-2, 3-dicarboxylic acid bis [(5-chloro-pyridine-2-yl)-amide] pure product.
Description
technical field [0001] The present invention relates to a method for preparing zopiclone impurities, in particular to a method for preparing pyrazine-2,3-dicarboxylic acid bis[(5-chloro-pyridin-2-yl)-amide]. [0002] technical background [0003] Zopiclone chemical name is 6-(5-chloropyridin-2-yl)-7-[(4-methylpiperazin-1-yl)carbonyloxy]-5,6-dihydropyrrole[ 3.4-b]pyrazin-5-one, a pyrrolidone compound, is the third-generation sedative-hypnoticdrug developed by the French Rhone-Poulene Rorer company. It is an inhibitory neurotransmitter γ- Aminobutyric acid (GABA) receptoragonist, with hypnotic, sedative, muscle relaxant, anxiolytic and anticonvulsant effects, mainly used for short-term treatment of insomnia caused by various reasons. [0004] Eszopiclone (Eszopiclone) is a fast-acting, short-acting non-benzodiazepinesedative and hypnoticdrug developed by Seprator Company in the United States. It was launched in the United States in April 2005 and belongs to the (S) isomer ...
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