37 results about "Dichloroquine" patented technology

The invention provides an industrial production method for hydroxychloroquine sulfate, which includes the following steps: enabling 4.7-dichloroquinoxaline and 5-(N-ethyl-N-ethoxyl)-2-amino pentane to react under gas shield for 13-24 h at a gradually increased temperature of 120-130 DEG C to obtain hydroxychloroquine; preparing the hydroxychloroquine sulfate after the reaction between the hydroxychloroquine and an alcohol sulfate solution at the temperature of 20-30 DEG C. According to the method, the yield of the obtained crude product of the hydroxychloroquine is not smaller than 85%, the yield of the obtained hydroxychloroquine sulfate is not smaller than 85%, the yield of the obtained hydroxychloroquine sulfate HPLC is not smaller than 99.5%, the yield of single impurity is not larger than 0.1%, so that requirements of United States Pharmacopeia is met; the novel method is simple in procedure, is environment-friendly and easy in industrial production.

The invention discloses a preparation process of chloroquine phosphate. The preparation process of the chloroquine phosphate comprises the following steps of: (1) taking 4, 7-dichloroquinoline as an initial raw material, carrying out condensation reaction with 2-amino-5-diethylaminopentane, and carrying out alkalization extraction to obtain chloroquine; and (2) salifying the chloroquine obtained in the step (1) with phosphoric acid to obtain chloroquine phosphate. The invention provides a preparation process of chloroquine phosphate. In the preparation process, the use of organic solvents suchas benzene and other catalysts such as phenol is avoided, and a condensation crystallization impurity removal step is introduced, so that the product purity is high, the individual impurity is less than 0.1%, the green chemical requirements and pharmacopeia standards are met, the operation is simple and convenient, the process is simplified, the production efficiency is improved, and the method is suitable for industrial production.

The invention provides a novel asymmetric synthesis method of (S) chloroquine. According to the invention, 5-(N-diethylamino)-2-pentanone and (S)-alpha-methyl benzylamine are adopted as raw materials,and in the presence of Lewis acid, an asymmetric reductive amination reaction is carried out to obtain (S,S)-5-(N'-diethylamino)-N-((1-phenyl)ethyl)-2-pentylamine, catalytic hydrogenation is performed to remove benzyl to obtain a side chain (S)-5-(N'-diethylamino)-2-amyl amine for synthesizing chloroquine, the (S)-5-(N'-diethylamino)-2-amyl amine is condensed with 4,7-dichloroquinoline to obtain(S)-chloroquine, salifying is performed with phosphoric acid, and recrystallizing is performed to obtain (S)-chloroquine phosphate with ee value of more than 99%, wherein the the total yield of the four-step reaction exceeds 70%; and the preparation method is stable, reliable, economical, efficient and easy to industrialize.

The invention relates to a preparation method of hydroxychloroquine sulfate, and belongs to the technical field of medicine synthesis. According to the preparation method of hydroxychloroquine sulfate, 7-chloro-4-fluoroquinoline and 5-(N-ethyl-N-2-hydroxyethyl amine)-2-pentylamine are subjected to a reaction to prepare hydroxychloroquine, and then hydroxychloroquine and sulfuric acid are salifiedto prepare hydroxychloroquine sulfate. The 7-chloro-4-fluoroquinoline is prepared from 4,7-dichloroquinoline through a halogen exchange reaction. The preparation method of hydroxychloroquine sulfate has the advantages of low reaction temperature, short reaction time, fewer byproducts, simple technique and favorable reproducibility, and is beneficial to industrial production.

The present invention provides a herbicidal composition containing quinocazone, the active components comprising quinocazone, penoxsulam and oxaflutole; and quinocazone, penoxsulam and The mass ratio of oxaflutole is 5-20:0.3-0.9:0.4-1.5; the composition of the invention has obvious synergistic effect, and the control effect is higher than that of a single agent; it can be used for the control of annual weeds in paddy fields.

The invention discloses a class of 6,7-dichloroquinoline-5,8-dione derivative transition metal complexes and a synthesis method and application thereof. The complex of the present invention has the structure shown in the following formula (I), and its synthesis method is to put metal nitrate and the compound shown in the following formula (II) in a mixed solvent, and carry out coordination under heating or without heating reaction, the reactant is cooled, allowed to stand, volatilized, and crystals are precipitated to obtain the target compound; wherein, the mixed solvent is a composition of methanol or ethanol and dichloromethane; the complex of the present invention is effective for certain tumor cells The strain has significant inhibitory activity and has low toxicity to normal human liver cells. The compounds shown in the formula (I) and the formula (II) are respectively as follows: wherein, M represents a divalent metal element selected from the fourth period of the periodic table; R represents H or CH 3 , X means H 2 O, CH 3 OH or CH 3 CH 2 Oh.

The invention provides a mixed herbicide containing propyrisulfuron and dichloroquinolone and an application thereof. The mixed herbicide contains active components of the propyrisulfuron and the dichloroquinolone; the weight ratio of the propyrisulfuron to the dichloroquinolone is 1-10:1-40. The mixed herbicide provided by the invention can be used for controlling broadleaf weeds, gramineous weeds and nutgrass flatsedge.

The invention relates to a preparation method of 4,7-dichloroquinoline in the technical field of medicine, which uses 2-amino-6-chlorobenzoic acid (I) as a starting material, and ethoxymethine in an organic solvent Diethyl malonate (II) undergoes condensation reaction to obtain (Ⅲ), III undergoes cyclization, hydrolysis, and acidification to obtain hydroxyquinoline dicarboxylic acid (V), V undergoes high-temperature decarboxylation to obtain hydroxyquinoline (VI), and VI undergoes Chlorination of phosphorus oxychloride gives 4,7-dichloroquinoline. The 4,7-dichloroquinoline prepared by the method of the present invention does not have the isomer 4,5-dichloroquinoline, and the temperature of the condensation reaction under the catalysis of the catalyst is low, which improves the yield of the reaction and avoids the generation of impurities , and reduce energy consumption, improve the economic benefits of the product.

The invention provides a preparation method of hydroxypiperaquine and phosphate thereof. The preparation method of hydroxypiperaquine comprises the following steps: by using piperazine, 1,3-dihalopropanol and 4,7-dichloroquinoline as raw materials, reacting the piperazine and 1,3-dihalopropanol by using an acid-binding agent as a catalyst to obtain 1,3-dipiperazinylpropanol, carrying out condensation reaction on the 1,3-dipiperazinylpropanol and 4,7-dichloroquinoline under the catalytic action of an alkali to obtain the hydroxypiperaquine. The obtained hydroxypiperaquine reacts with phosphoric acid to obtain the hydroxypiperaquine phosphate. The method has the advantages of mild reaction conditions, simple preparation technique and low cost, and is suitable for industrial production. The total reaction yield of the hydroxypiperaquine is up to 90-91.5%, and the total reaction yield of the hydroxypiperaquine phosphate is up to 82.7-87.5%.

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 present invention relates to the technical field of compound synthesis, and discloses a 4, 7-dichloroquinoline synthesis purification method, which comprises: S1, primary reaction: adding 7-chloro-4-hydroxyquinoline into 300 g of toluene, sequentially adding DMF and triphenylphosphine oxide, starting stirring, internally heating to a temperature of 79-90 DEG C, slowly adding phosphorus oxychloride or a toluene solution of phosphorus oxychloride in a dropwise manner, after the dropwise adding is completed, carrying out a reaction for 2-3 h, and cooling to a room temperature to obtain the 4, 7-dichloroquinoline. Continuously reacting until the TLC monitoring reaction is finished; s2, performing reduced pressure distillation, namely performing reduced pressure distillation on the reaction liquid in the S1. The method has the advantages of simple operation, high yield, no use of any reagent in the purification process, no introduction of new impurities, no special requirements on equipment, no environmental pollution, no introduction of an organic solvent, no pollution, and easy industrial production.

The invention belongs to the field of drug synthesis, and specifically relates to a new method for preparing 2,3-dichloroquinoxaline derivatives in one pot. Friendly silica gel or methanesulfonic acid is used as the catalyst, and the intermediate separation and purification steps are omitted, the operation is simple, the cost is low, the reaction conditions are mild, and it is environmentally friendly, and it is easy to industrialize large-scale production.