- Preparation process of pyridinone ethanol amine salt
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The invention relates to the technical field of pyridone ethanol amine salt processing, and particularly discloses a pyridone ethanol amine salt preparation process, which comprises: carrying out an acylation reaction, a ring-closure reaction, a hydroxyamination reaction and a salt forming reaction on 3,3-dimethyl acrylate and isononyl chloride to obtain pyridone ethanol amine salt; wherein the acylation reaction is carried out in the presence of a supported catalyst, the supported catalyst comprises an active component and a carrier, the carrier is silica gel, the active component comprises anhydrous aluminum chloride, anhydrous lanthanum chloride and anhydrous lithium perchlorate, and the loading capacity of anhydrous aluminum chloride on the carrier is 7-11 wt%; the loading capacity ofanhydrous lanthanum chloride on the carrier is 3-5 wt%; and the loading capacity of anhydrous lithium perchlorate on the carrier is 0.8-1.5 wt%. According to the preparation process of pyridinone ethanol amine salt, the catalytic Friedel-Crafts acylation reaction is realized, the supported catalyst is convenient to recover, and the activity and selectivity of the supported catalyst are improved.
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Paragraph 0049; 0051; 0060; 0061; 0064; 0073-0074; 0077-0087
(2021/01/25)
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- Synthetic method of pyridone ethylamine salt
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The method comprises the following steps: S1 adding isononyl chloride, Lewis acid and 3,3 -dimethyl acrylate into a container to perform a Fourier acylation reaction to obtain an intermediate M1. S2 of an intermediate M1, hydroxylamine hydrochloride and 0 - 140 °C was added to a solvent to perform cyclization and hydroxyamination reaction to obtain an intermediate M2. S3 intermediate M2 is salified with ethanolamine to give a pyridone ethylamine salt. Compared with the prior art, two reaction systems of lactone and hydroxypipone are obtained by hydroxyamination, and the method for synthesizing the pyridone ethylamine salt is simplified. The reaction system has the advantages of low temperature, low requirement on process and equipment, safety in reaction conditions, simple and convenient operation, and suitableness for industrial mass production. There is no need to use concentrated sulfuric acid. Acetic acid, alkali, catalyst, safety and environmental protection, reduce cost.
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Paragraph 0037; 0040-0041; 0047; 0050-0051; 0054; ...
(2021/11/06)
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- Preparation method of pyridinone ethanolamine salt
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The invention discloses a preparation method of a pyridinone ethanolamine salt. The preparation method comprises the reaction steps of Friedel-Crafts acylation, ring closing, hydroxyamination, salification and the like. According to the preparation method, the pyridinone ethanolamine salt can be efficiently prepared under mild conditions, less reaction materials are consumed, the yield and purityof products obtained in the steps are high, and complex purification steps are not needed.
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Paragraph 0050-0051; 0054; 0056; 0059; 0061; 0064; 0066
(2020/03/05)
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- Continuous synthesis method of piroctone
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The invention relates to a continuous synthesis method of piroctone. The method comprises the following steps: providing a first solution and a second solution; and respectively and continuously pumping the first solution and the second solution into a microreactor, and reacting at the temperature of 90-180 DEG C and the pressure of 0.2-2MPa to obtain the piroctone. According to the synthesis method of the piroctone, potassium tert-butoxide is used as a catalyst and an alkali, isopropanol is used as a solvent, and a continuous synthesis process is realized by adopting the microreactor, so thatthe yield of the piroctone can reach more than 85%, the reaction time is shortened to be within 60 minutes, and the production cycle is shortened. Besides, the microreactor system is closed, so thatcontact reaction between hydroxylamine and oxygen, moisture and the like in the external environment is avoided, side reaction and loss of the hydroxylamine are greatly reduced, and the post-treatmentprocess is simpler and safer.
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Paragraph 0049-0105
(2020/04/17)
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- PROCESS FOR FORMING 2-HYDROXYPYRIDINE-1-OXIDE OR DERIVATIVES THEREOF
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A process for forming 2-hydroxypyridine-1 -oxide or derivatives thereof, the process comprising inter alia providing a solution comprising at least one compound according to Formula (1) (I) and recovering a compound according to Formula (2) (2) Also related products, uses, methods and compositions.
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Page/Page column 88; 89
(2019/12/25)
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- The chemistry of antimicrobially active 1-hydroxy-2-pyridones
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The unsaturated δ-keto esters obtained by condensation of acid chlorides with esters of di- or trialkyl-acrylic acids can be cyclized with hydroxylamine to yield 1-hydroxy-2-pyridones. However, in many cases a two-steps synthesis may be of advantage in preparative respect, the ketoesters being cyclized to 2-pyrones, which then are reacted with hydroxylamine in the presence of certain bases to give. The hydroxy-pyridones show pronounced antifungal activity in vitro as well as in experimental guinea pig dermatophytosis.
- Lohaus,Dittmar
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p. 1311 - 1316
(2007/10/02)
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- Process for the preparation of 1-hydroxy-pyridones
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Method for making 6-substituted-1-hydroxy-2-pyridones, which may also be substituted in one or more of the 3-, 4-, and 5-positions, by reaction of the corresponding 2-pyrone with hydroxylamine or its salts in the presence of imidazole or a 2-aminopyridine which may be mono- or di-methyl substituted.
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