The "6-Amino-1,3-dimethyl uracil Market" reached a valuation of USD xx.x Billion in , with projections to achieve USD xx.x Billion by , demonstrating a compound annual growth rate (CAGR) of xx.x% from to .
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Global 6-Amino-1,3-dimethyl uracil Market Dynamics
6-Amino-1,3-dimethyl uracil Market Trends
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Short Description About 6-Amino-1,3-dimethyl uracil Market:
Key insights provided include market and segment sizes, competitive landscapes, current status, and emerging trends. Additionally, the report offers in-depth cost analyses and supply chain evaluations.
Technological innovations are anticipated to enhance product performance, driving broader adoption across various downstream applications. Furthermore, insights into consumer behavior and market dynamics, including drivers, restraints, and opportunities, furnish vital intelligence for understanding the 6-Amino-1,3-dimethyl uracil Market landscape.
6-Amino-1,3-dimethyl uracil Market Segments Analysis
The 6-Amino-1,3-dimethyl uracil Market research report employs a meticulous segmentation strategy, offering deep insights into various market segments such as application, type, and region. This approach provides readers with a nuanced understanding of the driving forces and obstacles within each segment, tailored to meet the discerning needs of industry stakeholders.
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Detailed TOC of Global 6-Amino-1,3-dimethyl uracil Market Research Report, -
1. Introduction of the 6-Amino-1,3-dimethyl uracil Market
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2. Executive Summary
3. Research Methodology of Verified Market Reports
4. 6-Amino-1,3-dimethyl uracil Market Outlook
5. 6-Amino-1,3-dimethyl uracil Market, By Product
6. 6-Amino-1,3-dimethyl uracil Market, By Application
7. 6-Amino-1,3-dimethyl uracil Market, By Geography
8. 6-Amino-1,3-dimethyl uracil Market Competitive Landscape
9. Company Profiles
10. Appendix
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Technical field
The invention belongs to Synthetic Organic Chemistry technical field, be specifically related to a kind of 6-chloro-1,3-FU dimethyl inovel preparation method.
Background technology
6-is chloro-1,3-FU dimethyl iit is the important intermediate of synthetic Altace Ramipril urapidil (urapidil) and antiarrhythmic drug Nifekalant (nifekalant).
Urapidil is by Byk Gulden company, to develop first the depressor of listing in , at present in the listing of more than 30 state approval such as English, method, and the clinical primary renal hypertension, pheochromocytoma and in heart failure etc. of being used for the treatment of.This medicine is the depressor with periphery and maincenter activity of first listing, the α on human peripheral blood pipe unstriated muscle and SNE postsynaptic membrane 1-acceptor has retardation, and direct excited brain stem 5-HT 1Aacceptor, produces central hypotensive effect.China this medicine of import for many years, is widely used clinically.
Nifekalant is the novel I II class anti-arrhythmic going on the market in Japan first in , belong to non-selective potassium channel antagonist, the quick ventricular arrhythmia that can effectively control turns back causes, ischemic arrhythmia is had to good curative effect, there is safer, broad-spectrum high efficacy more compared with other antiarrhythmic drug.
Relevant 6-is chloro-1,3-FU dimethyl isynthetic, on document, only there is the condensation in acetic acid/aceticanhydride of Dimethylurea and propanedioic acid first to make 1,3-dimethyl barbituric acid, then the method for preparing through phosphorus oxychloride chlorination, as United States Patent (USP) 4,659,651() report technique, two step yields are respectively 73.6% and 65.0%, total recovery only 47.8%, and propanedioic acid, aceticanhydride, phosphorus oxychloride large usage quantity, aftertreatment is loaded down with trivial details, and cost is higher.Wang Yalou etc. (Chinese Journal of Pharmaceuticals ,33(1), 521-523) reported similar synthetic method, 1,3-dimethyl barbituric acid is without separation, and directly and phosphorus oxychloride chlorination, total recovery increases, and reaches 63.3%.
Existing technique chlorinating step exists yield low, and the shortcomings such as operational difficulty cause production cost higher, and quality product is not high.
Summary of the invention
It is chloro-1 that the present invention aims to provide a kind of easy handling, 6-that yield is higher, 3-FU dimethyl preparation method.
The present invention is with 6-amino-1,3-FU dimethyl iIIfor raw material, through acid hydrolysis, make 6-hydroxyl-1,3-FU dimethyl iI, then it is chloro-1 through chlorination, to make 6-, 3-FU dimethyl i, being wherein hydrolyzed yield more than 90%, chlorination yield is more than 80%, and two step total recoverys reach more than 70%, are significantly higher than literature method.Its raw material 6-amino-1,3-FU dimethyl iIIcan by Dimethylurea and cyanoacetic acid condensation, be prepared easily, mild condition, yield is very high, and all more than 90%, and cyanoacetic acid price is low, it is excessive not need, so help (Chinese Journal of Pharmaceuticals ,31(7) such as monarchs 294-296), (Chinese Journal of New Drugs such as Fu Ye, 13(6), 538-539) etc. the technique reported.
Synthetic route of the present invention is as follows:
III II I
Hydrolysis reaction in the present invention can reference literature method carry out, the optional phosphoric acid of mineral acid, sulfuric acid, hydrochloric acid, Hydrogen bromide, nitric acid etc., organic acid can be methylsulfonic acid, formic acid, acetic acid, trifluoroacetic acid etc., all can obtain good result, the optional methyl alcohol of solvent, ethanol, Virahol, water, or the mixture of alcohol and water, 60 &#;&#;120 &#; of temperature of reaction, reaction times 1h&#;10h.
Though the chlorination reaction in the present invention can reference literature method be carried out, and selects phosphorus pentachloride, phosphorus pentachloride adds phosphorus oxychloride, phosphorus oxychloride, phosphorus trichloride adds phosphorus oxychloride, trichloromethylchloroformate, triphosgene, oxalyl chloride, sulfur oxychlorides etc., add or do not add simultaneously DMA, N, dinethylformamide etc., but chlorination yield is all no more than 65%.
Intermediate iIduring chlorination, the strict anhydrous condition of general requirement, therefore generally can not add additive easy and that phosphorus oxychloride reacts.But present inventor is surprisingly discovery but, iIchlorination time, conventional additive does not have great role, and adds a small amount of alcohol, particularly water has very large promoter action to reaction, yield can be increased to more than 80% by 65%, and aftertreatment is also simplified. iIwith the mol ratio of additive be 1.0:0.05&#;0.5, but additive can not add in reactor in advance, and must slowly splash at low temperatures in phosphorus oxychloride.
The present invention is by 6-amino-1, and it is chloro-1 that 3-FU dimethyl makes 6-through two-step reaction, 3-FU dimethyl, and reaction conditions gentleness, method is easy, and product yield is high, and cost is low, raw materials used cheap and easy to get.The above-mentioned effect of the inventive method provides good prospect for suitability for industrialized production.
Embodiment
Embodiment 1 adds 6-amino-1 in L reactors, 3-FU dimethyl 150 &#;, water 600 &#;, the vitriol oil (98%) 50 &#;, be heated to gradually backflow, keep 5 hours, crystallisation by cooling, centrifugal, be dried to obtain oyster white crystallization 6-hydroxyl-1,3-FU dimethyl 140.5 &#;, 121 &#;-124 &#; of fusing points, yield 93.0%.In 500 L dry reaction stills, suction 450 &#; phosphorus oxychloride and 150 &#; phosphorus trichlorides respectively, be cooled to below 20 &#;, slowly drip water 14 &#;, drip to finish and add 6-hydroxyl-1 that totally 50 &#; as above make in batches, 3-FU dimethyl, after adding, be warming up to gradually backflow, be incubated after 3 hours and stop heating, slowly squeeze into vacuum, start reclaim under reduced pressure phosphorus oxychloride, when becoming muddy, material in 90 &#; of left and right stills stops distillation, turn while hot material to being added with in the still of 500 &#; frozen water in advance, control 60 &#; of following hydrolysis, 15-30 minute is stirred in complete continuation, be cooled to below 40 &#;, adjust pH=2&#;3 with liquid caustic soda, temperature control is in 40 &#;.Stir 10 minutes, be cooled to below 30 &#;, centrifugal solid crude product 47 &#; that obtain, content is more than 98%.This crude product adds water 100 &#;, methyl alcohol 80 &#;, and gac 3 &#;, reflux decolour, filters, and crystallisation by cooling is centrifugal, dries to such an extent that fine work 6-is chloro-1,3-FU dimethyl 44.9 &#;, content 99.2%, fusing point 113-114 &#;, yield 80.3%.
Embodiment 2 adds 6-amino-1 in L reactors, 3-FU dimethyl 150 &#;, water 400 &#;, concentrated hydrochloric acid (36%) 150 &#;, is heated to backflow gradually, keeps 4 hours, be cooled to 30 &#; of following crystallizations, centrifugal, mother liquor is refrigerated to below 10 &#;, separate out solid, centrifugal, be dried to obtain off-white color crystallized product 6-hydroxyl-1,3-FU dimethyl 139 &#;, 121 &#;-124 &#; of fusing points, yield 92.0%.In 500 L dry reaction stills, suction 600 &#; phosphorus oxychloride, be cooled to below 20 &#;, slowly drip methyl alcohol 20 &#;, drip to finish and add 6-hydroxyl-1 that totally 50 &#; as above make in batches, 3-FU dimethyl, after adding, be warming up to gradually backflow, be incubated after 5 hours and stop heating, slowly squeeze into vacuum, start reclaim under reduced pressure phosphorus oxychloride, when becoming muddy, material in 90 &#; of left and right stills stops distillation, turn while hot material to being added with in the still of 800 &#; frozen water in advance, control 60 &#; of following hydrolysis, 15-30 minute is stirred in complete continuation, be cooled to below 40 &#;, with sheet adjusting PH with base=2&#;3, temperature control is in 40 &#;.Stir 10 minutes, be cooled to below 30 &#;, centrifugal solid crude product 48 &#; that obtain, content is more than 98%.This crude product adds water 100 &#;, acetone 100 &#;, and gac 3.5 &#;, reflux decolour, filters, and crystallisation by cooling is centrifugal.Dry to such an extent that fine work 6-is chloro-1,3-FU dimethyl 45.3 &#;, content 99.3%, fusing point 113-114 &#;, yield 81.0%.
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