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A technology for iodixanol hydrolyzate and substance, which is applied in the preparation of organic compounds, the preparation of carboxylic acid amides, chemical instruments and methods, etc., can solve the problem of low yield, reduced reaction yield, difficult scale industrial production, etc problems, to achieve the effect of improving yield, reducing environmental pollution, and simplifying production operations
Active Publication Date: 2008-06-11
ZHEJIANG HAIZHOU PHARMA CO LTD
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In this synthetic route, because the dichlorination reaction time is too long, the reaction yield is reduced
And when reacting with 1-amino-2,3-propanediol and acetic anhydride, crystallization of the product is difficult, the yield is not high, and it is difficult to carry out large-scale industrial production;
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Embodiment 1
[0033] In a 1000 ml reaction flask, add 59.9 g (0.1 mol) of 5-acetylamino-2,4,6-triiodo-1,3-benzenedicarboxamide, 16.6 g (0.15 mol, 13.6 ml) of α-chloroglycerol , a catalytic amount of pyridine, 300 milliliters of 1-butyl-3-methylimidazolium tetrafluoroborate, heated up to 100 ° C, stirred, and reacted for 4 hours. After the reaction was completed, cooled to room temperature and post-treated to obtain 67 grams of the product. Yield 90%.
Embodiment 2
[0035] In a 1000 ml reaction flask, add 59.9 g (0.1 mol) of 5-acetylamino-2,4,6-triiodo-1,3-benzenedicarboxamide, 11 g (0.1 mol, 9 ml) of α-chloroglycerol , a catalytic amount of triethylamine, 300 ml of 1-butyl-3-methylimidazolium tetrafluoroborate, heated up to 100°C, stirred, and reacted for 4 hours. After the reaction was completed, cooled to room temperature and post-processed to obtain the product 62 grams, yield 83%.
Embodiment 3
[0037] In a 1000 ml reaction flask, add 59.9 g (0.1 mol) of 5-acetylamino-2,4,6-triiodo-1,3-benzenedicarboxamide, 16.6 g (0.15 mol, 13.6 ml) of α-chloroglycerol , a catalytic amount of pyridine, using 300 ml of 1-butyl-3-methylimidazolium tetrafluoroborate, heated up to 100 ° C, stirred, and reacted for 4 hours. After the reaction was completed, cooled to room temperature and post-processed to obtain the product 67 grams, yield 90%.
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Abstract
The invention provides a method for preparing 5-(acetylamino)-N, N'-di (2, 3-dihydroxy propyl)-2, 4, 6-triiodide-1, 3-phenyl diformamide as Iodixanol hydrolysate and the method is that 5-acetylamino-2, 4, 6-triiodide-1, 3-phenyl diformamide is adopted as raw material to react with alpha-halogenated glycerin or 1-halogenated-2, 3-epoxypropane under the temperature of 30-150 DEG C for 1-20 h in the molecular organic solvent or ion liquid such as alkyl benzene, DMSO, DMF, acetonitrile, C1-C10 alcohol and the like acted by inorganic or organic alkaline such as catalyst quantity of alkaline metal carbonate, alkaline hydroxide, organic amine and the like. The obtained material is separated and purified to produce Iodixanol hydrolysate. The invention has the advantages of simplifying production operation, fitting for industrial batch production, reducing environmental pollution, improving the yield, thereby reaching the goal of reducing energy consumption.
Description
(1) Technical field [0001] The invention relates to a hydrolyzate of iodixanol: 5-(acetylamino)-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzene The preparation method of diformamide. (2) Background technology [0002] Iodixanol hydrolyzate: 5-(acetylamino)-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide (NA -ATIBA-A), is the key intermediate of the non-ionic monomer contrast agent iohexol, and is also an important intermediate for the synthesis of the non-ionic dimer contrast agent iodixanol, and is the most commonly used in interventional radiology operations One of the drugs, mainly used for the display of blood vessels and body cavities. There are various types of contrast agents, and most of the contrast agents used in interventional radiology are iodine-containing preparations, which have broad application prospects. [0003] In recent years, in many countries in the world, the contrast agent market has shown a trend of vigorous developme...
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