37 results about "Dichloroquine" patented technology

The invention discloses a process for preparing Quinclorac artificial semiantigen, artificial antigen, specific antibody and use thereof, wherein the preparation comprises, subjecting the dichloroquine (3,7-dichlorine-8-quinoline carboxylic acid) to sulfoxide chlorinated acylation, reacting with reanal and aminocaproic acid, thus obtaining semiantigen 4-(3,7-dichlorine-8-quinolineformyl) reanal or 6-(3,7-dichlorine-8-quinolineformyl) aminocaproic acid (QB or QC).

The invention relates to the field of herbicides, and discloses a preparation method of quinclorac, which comprises: 1) adopting an N-hydroxyphthalimide compound and azodiisobutyronitrile as catalysts, adopting oxygen as an oxidizing agent, and oxidizing 7-chloro-8-methylquinoline to obtain 7-chloro-8-quinoline carboxylic acid; and 2) by taking azodiisobutyronitrile as a catalyst, carrying out chlorination reaction on 7-chloro-8-quinoline carboxylic acid and chlorine to obtain 3,7-dichloro-8-quinoline carboxylic acid. By means of the method disclosed by the invention, the generation of a largeamount of waste acid and wastewater in a synthesis process can be reduced, and the product yield of quinclorac can be increased.

The invention discloses hydroxychloroquine sulfate and a preparation method thereof, and relates to the technical field of medicinal chemistry. The preparation method comprises the steps of mixing 4, 7-dichloroquinoline with a hydroxychloroquine side chain, carrying out heating condensation in the presence of an organic base catalyst, adding water and liquid, and carrying out cooling crystallization to obtain hydroxychloroquine; and dissolving hydroxychloroquine in an ethyl acetate and ethanol aqueous solution, heating, dissolving and clarifying, dropwise adding concentrated sulfuric acid, cooling, crystallizing, filtering and drying to obtain hydroxychloroquine sulfate. The method has the beneficial effects that a solvent-free reaction is used, and a catalyst is added, so that high pollution is avoided, the reaction process is accelerated, and the operation is simple; and meanwhile, the HPLC purity of the obtained hydroxychloroquine refined product is not less than 96.50%, the maximum single impurity content is less than 0.10%, the yield can reach 85%, the HPLC purity of hydroxychloroquine sulfate is not less than 98.00%, the maximum single impurity content is less than 0.10%, and the yield can reach 90%.

The invention discloses a preparation method of chloroquine phosphate, namely 7-chloro-4-(4-diethylamino-1-methylbutylamino)quinoline diphosphate. The preparation method comprises the following steps: (1) carrying out a condensation reaction on 4,7-dichloroquinoline and 2-amino-5-diethylaminopentane, and carrying out alkalization extraction, concentration and crystallization to obtain chloroquine; and (2) salifying the chloroquine obtained in the step (1) and phosphoric acid to obtain chloroquine phosphate. The method avoids the use of phenol, is simple in reaction, and is beneficial to industrial production; and the chloroquine is crystallized to improve the purity and then salified with the phosphoric acid, so product appearance is good, the purity of the produced chloroquine phosphate is greater than or equal to 99.5%, and a single impurity is less than 0.1% (according to an HPLC area normalization method).

The invention relates to a synthesis method of 3-ethyl carboxylate-4-chloro imidazole [1,5-a] quinoxaline, which is mainly used for solving the technical problems of the existing scarce synthetic route, expensive reaction raw materials, difficulty in amplification, narrow application range and the like. The synthesis method comprises the following steps: heating o-phenylenediamine 1 which is a cheap and available chemical raw material and diethyl oxalate for reacting in a solvent to obtain a compound 2 which is 2,3-dihydroxyl quinoxaline; heating the compound 2 and a chloride reagent for reacting to obtain a compound 3 which is 2,3-dichloro-quinoxaline; and reacting the compound 3 with ethyl isocyanoacetate in a solvent in the presence of an alkalization reagent to obtain the final product, namely 3-ethyl carboxylate-4-chloro imidazole [1,5-a] quinoxaline. By adopting the synthetic route provided by the invention, a large quantity of the 3-ethyl carboxylate-4-chloro imidazole [1,5-a] quinoxaline can be quickly and conveniently prepared.

The invention relates to a preparation method of 4, 7-dichloroquinoline in the technical field of medicines, and the method comprises the following steps of: carrying out condensation reaction on 2-amino-6-chlorobenzoic acid (I) serving as an initial raw material and diethyl ethoxymethylenemalonate (II) in an organic solvent to obtain (III), and carrying out cyclizing, hydrolyzing and acidifying on (III) to obtain hydroxyquinoline dicarboxylic acid (V). performing high-temperature decarboxylation on V to obtain hydroxyquinoline (VI), and chlorinating VI with phosphorus oxychloride to obtain 4,7-dichloroquinoline. The 4, 7-dichloroquinoline prepared by the method disclosed by the invention does not contain isomer 4, 5-dichloroquinoline, and the temperature of the condensation reaction is low under the catalysis of the catalyst, so that the reaction yield is improved, the generation of impurities is avoided, the energy consumption is reduced, and the economic benefit of the product is improved.

The invention discloses a weeding composition containing dichloroquinoline oxadiazon. Active components of the weeding composition containing dichloroquinoline oxadiazon comprise dichloroquinoline oxadiazon, bentazone and cyhalofop-butyl. According to the weeding composition disclosed by the invention, due to different weeding mechanisms of dichloroquinoline oxadiazon, bentazone and cyhalofop-butyl, the complex synergism effect of dichloroquinoline oxadiazon, bentazone and cyhalofop-butyl is obvious, and the herbicide controlling spectrum is wide; the weeding composition containing dichloroquinoline oxadiazon is relatively good in prevention and treatment effect on broadleaf weeds, cyperus weeds and gramineous weeds; the drug use amount is reduced, so that the cost is reduced, and the weeding composition is safer; meanwhile, the drug resistance generated by the use of a single dosage can be relieved.

The invention is directed to a method or use of 2,9-dichloro-quinacridone as a crystal phase inhibitor during the beta-quinacridone or gamma-quinacridone crude pigment particle size reduction processes. 2,9-dichloroquinacridone is added to the milling composition of the crude gamma or crude beta quinacridone

The invention discloses a preparation method of hydroxychloroquine sulfate, and belongs to the technical field of medicine synthesis. The method comprises the following steps: (1) mixing 4, 7-dichloroquinoline, an auxiliary agent and phenol, heating, adding a side chain, and reacting to obtain a hydroxychloroquine crude product; (2) purifying the hydroxychloroquine crude product obtained in the step (1) to obtain hydroxychloroquine; and (3) dissolving the hydroxychloroquine obtained in the step (2), and adding sulfuric acid to obtain hydroxychloroquine sulfate. The preparation method can shorten the reaction time, reduce the reaction temperature, reduce the generation of impurities, greatly reduce the production cost and reduce the environmental pollution, and is simple to operate and suitable for industrial production.

The invention discloses a new synthesis process of a quizalofop-ethyl pesticide intermediate high-purity 2-(4-hydroxyphenoxy)-6-chloroquinoxalin. The synthesis process comprises the following steps of: adding 2, 6-dichloroquinoxaline and hydroquinone into a mixed solvent; heating the mixed solvent, and dripping liquid alkali; carrying out thermal insulation reaction after dripping, separating out an organic solvent after reaction; and cooling, discharging and washing to obtain a high-purity target. With the adoption of the process, the excess ratio of hydroquinone and the sewage production difficulty are greatly lowered. The new synthesis process is a green process.

The invention provides a method for synthesizing optically pure (R)/(S)-hydroxychloroquine, which comprises the following steps: resolving (+/-)-2-[(4-aminoamyl)ethylamino]ethanol by using a resolving reagent, recrystallizing and purifying the compound to obtain optically pure (R)/(S)-2-[(4-aminoamyl)ethylamino]ethanol; and reacting the obtained single-configuration hydroxychloroquine side chain with 4,7-dichloroquinoline to obtain the hydroxychloroquine sulfate of single configuration. The method has the advantages of simple route, easily available raw materials, high yield, good stereoselectivity (ee% is greater than 99%), simple operation, greenness and environmental protection, and is suitable for large-scale production.

The invention discloses a preparation method of naphthoquine phosphate formula I. The preparation method is characterized by comprising the following steps: reacting p-aminophenol formula VI with 1, 4-disubstituted butane formula V to obtain 4-amino-5, 6, 7, 8-tetrahydro-1-naphthol formula IV, and reacting the formula IV with 4, 7-dichloroquinoline formula VII to obtain 4-(7-chloro-4-quinoline amino)-5, 6, 7, 8-tetrahydro-1-naphthol formula III, reacting the formula III with formaldehyde and tert-butylamine to obtain naphthoquine basic formula II, and salifying the naphthoquine basic formula II with phosphoric acid to obtain naphthoquine phosphate formula I; the process route has the advantages of simple and accessible raw materials, high yield and low pollution and is suitable for industrial production.