- Benzalkonium chloride preparation method
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The invention discloses a benzalkonium chloride preparation method, which comprises: (1) carrying out a salt formation reaction on a fatty alkyl dimethyl tertiary amine and benzyl chloride in an organic solvent at a temperature of 30-70 DEG C to obtain fatty alkyl dimethyl benzyl ammonium chloride, wherein the fatty alkyl is dodecyl, tetradecyl or hexadecyl, and the organic solvent is one or a plurality of materials selected from methanol, ethanol, n-propanol, isopropanol, acetone and acetonitrile; and (2) in an organic solvent, crystallizing the mixture containing two or three fatty alkyl dimethyl benzyl ammonium chlorides prepared in the step (1). According to the present invention, the preparation method has advantages of simple process and high yield, wherein the yield can achieve morethan 90%; the content of the related substance is low, and the purity is high, and can achieve more than 99%; the water content is low; and the product has good appearance and simple post-treatment effect, can meet the requirements of various pharmacopoeia, and is suitable for the industrial production of pharmaceutical-grade benzalkonium chloride.
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Paragraph 0069-0070
(2019/04/26)
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- Fatty alkyl dimethyl benzyl quaternary ammonium salt synthesis method
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The invention discloses a fatty alkyl dimethyl benzyl quaternary ammonium salt preparation method, which comprises: carrying out a salt formation reaction on fatty alkyl dimethyl tertiary amine and abenzyl halide in an organic solvent at a temperature of 30-70 DEG C, wherein R in the fatty alkyl tertiary amine is C6H13-C22H45, the halogen in the benzyl halide is chlorine, bromine or iodine, and the organic solvent is one or a plurality of materials selected from methanol, ethanol, n-propanol, isopropanol, acetone and acetonitrile. According to the present invention, the yield of the preparation method is high, and can reach more than 90%; the purity is high, and can achieve more than 99%; the water content is low; the product has good appearance and simple post-treatment effect; and the method can reduce the energy consumption, and is suitable for industrial production.
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Paragraph 0065; 0066; 0071; 0075
(2019/04/26)
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- Synthetic method of aryl sulphobetaine in solvent-free system
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The invention relates to a synthetic method of aryl sulphobetaine in a solvent-free system. The method comprises the steps that alkyl dimethyl tertiary amine and benzyl chloride which are close to the stoichiometric ratio react to synthetize alkyl dimethyl benzyl ammonium chloride at a low temperature, under high-speed stirring of a planetary stirrer and dilution of dry air in the solvent-free system, alkyl dimethyl benzyl ammonium chloride is added into chlorosulfonic acid close to the stoichiometric ratio step by step for a reaction, and alkyl dimethyl benzyl sulphobetaine is obtained. According to the method, no solvent is needed, the production cost is low, a small amount of residual chlorosulfonic acid obtained after a solvent-free reaction can be recycled through high-speed centrifugation, and the yield of alkyl dimethyl benzyl sulphobetaine can reach 98% or above.
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Paragraph 0028; 0029; 0045; 0046
(2017/04/03)
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- Benzalkonium chloride monomer synthesis technology
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The invention relates to the technical field of fine chemicals, and more specifically relates to a benzalkonium chloride monomer synthesis technology. The synthesis technology comprises the following steps: (1) according to a formula, weighing fatty alkyl dimethyl tertiary amines, benzyl chloride, and ethyl acetate; (2) adding ethyl acetate into a glass lined reactor, pumping fatty alkyl dimethyl tertiary amines and benzyl chloride into a head tank, starting the stirring device of the reactor, dropwise adding fatty alkyl dimethyl tertiary amines and benzyl chloride into the reactor at a room temperature according to a same ratio; (3) heating the reactor to a temperature of 70 to 100 DEG C, and maintaining the temperature to carry out reactions for 7 to 10 hours; (4) starting circulating cooling water to cool the products to the room temperature until crystals are precipitated completely; (5) taking out the crystals, subjecting the crystals to vacuum suction filtration, during the suction filtration process, washing the crystals by ethyl acetate for 2 to 5 times, and saving the filter cakes; and (6) adding ethyl acetate into the filter cakes, carrying out re-crystallization, and after the crystals are completely precipitated, drying the crystals. The production cost is low and the purity of prepared benzalkonium chloride is high.
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Paragraph 0016; 0021
(2017/09/01)
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- A synthetic method of a benzalkonium chloride mixture
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The invention relates to the technical field of organic synthesis, and particularly relates to a synthetic method of a benzalkonium chloride mixture. The method includes (1) weighing alkyl dimethyl tertiary amine, a metal or nonmetal halide, benzyl chloride and an organic solvent separately according to a ratio; (2) dissolving the alkyl dimethyl tertiary amine and the metal or nonmetal halide into the organic solvent according to a ratio to obtain a mixture system, putting the mixture system in a hydrothermal boiler and raising the temperature of the mixture system to 50-80 DEG C; (3) adding dropwise the benzyl chloride into the mixture system in the step (2) under continuous stirring, with the adding speed being 30-40 drops per min, stirring the mixture system until the dropwise addition is finished, and allowing the obtained mixture system to stand for 3-8 h to obtain benzalkonium chloride single crystals; and (4) subjecting the mixture system in the step (3) to suction filtration, and performing washing operation and recrystallization to obtain the benzalkonium chloride. Compared with traditional processes, the metal or nonmetal halide is adopted as an additive of the method, can promote benzalkonium chloride generation from a reaction of the alkyl dimethyl tertiary amine and the benzyl chloride, and increases the conversion ratio of reactants; and a benzyl chloride dropwise addition manner is adopted by the method, thus reducing benzyl chloride volatilization, allowing the benzyl chloride to be completely reacted as soon as the benzyl chloride is added into a solution, and increasing the conversion ratio of the reactants.
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Paragraph 0016; 0021; 0022
(2017/08/30)
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- STABLE COMPOSITIONS OF THIABENDAZOLE AND IODINE-CONTAINING FUNGICIDES
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The present invention relates to stable compositions for the fungicidal equipment of thermoplastic polymers, in particular PVC, comprising thiabendazole, at least one iodine-containing fungicide and at least one epoxide and optionally further fungicidally active compounds, and also to methods for preparing these formulations and to uses thereof for the protection of thermoplastic polymers against attack and destruction by microorganisms. Moreover, the invention relates to mold-resistant PVC materials equipped with the compositions according to the invention.
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- Synthesis of some acyclic quaternary ammonium compounds. Alkylation of secondary and tertiary amines in a two-phase system
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A series of acyclic symmetrical and asymmetrical quaternary ammonium chlorides of the general formula R1R2R3N+AR4Cl- (R1 = Me, Bu; R2 = n-C12H25, PhCH2, C n H2n+1(OCH2CH2) m, n = 9 and 12, m = 1 and 2; R3 = n-C12H25, PhCH2, HOCH2CH2,-OOCCH2; R4 = n-C12H25, PhCH2; A = (CH2CH2O)1,2, CH2C(O)O) was synthesized by the alkylation of tertiary amines in a two-phase system containing water. A convenient method for the synthesis of the initial symmetrical and asymmetrical tertiary amines of the general formula MeNR1R2 (R1 = Me, Bu; R2 = n-C12H25, PhCH2, CnH2n+1(OCH2CH2) m, n = 9 and 12, m = 1 and 2) in an organic phase-aqueous phase heterogeneous system, which allows the use of aqueous solutions of alkali and amines, was developed. The improved method for the preparation of intermediate ethylene glycol and diethylene glycol monoethers is monoalkylation of glycols in dioxane using solid KOH in a two-phase system.
- Kharlamov,Artyushin,Bondarenko
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p. 2445 - 2454
(2015/08/03)
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- ACTIVE DELIVERY SYSTEMS FORMULATIONS
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The present invention relates to active delivery system formulations, and methods of making and using the same. Said formulations, when applied to a substrate surface, form a protective coating on the surface and permit constituent active agents to act on the surface and in the surrounding medium.
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- DENTAL ORAL COMPOSITION
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A dental composition for oral use, containing a phosphorylated saccharide (a), a polyphosphoric acid and/or a salt thereof (b), and a cationic bactericidal agent (c), wherein a ratio of a total amount of the phosphorylated saccharide (a) and the polyphosphoric acid and/or a salt thereof (b) contained to an amount of the cationic bactericidal agent (c) contained, i.e. {(a)+(b)}/(c), is from 0.05 to 20 in a weight ratio. The dental composition for oral use of the present invention can be suitably used for an oral cavity cleaning agent, including dentifrice agents such as a paste dentifrice agent, a powder dentifrice agent, and a liquid dentifrice agent, a mouse-wash agent, a troche, a tablet, a cream, an ointment, a bonding agent, a mouth spray, a coating agent to tooth surface or a dental prosthetic, a hypersensitive inhibitor, a therapeutic agent for periodontal diseases, that is applied to a periodontal pocket, wet tissue for oral cavity care, an oral refreshing agent, chewing gum, or a gargling agent, or the like.
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- NOVEL FORMULATION OF DEHYDRATED LIPID VESICLES FOR CONTROLLED RELEASE OF ACTIVE PHARMACEUTICAL INGREDIENT VIA INHALATION
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A new formulation of dehydrated lipid vesicles employs a vesicle preserver and permits the control of release and delivery of active pharmaceutical ingredients into the respiratory system for treatment in particular of asthma. The typical formulation provides controlled release of the active pharmaceutical ingredient from 0% to 100% from 0 to 72 hours after inhalation, changes the systemic administration to topical administration, allows prolonged therapeutic period for one administration, increased stability, with reduced dose, reduced systemic side effects, reduced toxicity.
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- METHOD FOR PRODUCING ALKYLDIMETHYLBENZYLAMMONIUM CHLORIDES
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The invention is meant for chemical industry and is applicable in production of household sanitizers and detergents. A mixture of commercial tertiary amines or a mixture of straight-run tertiary amines is rectified and fed into the reactor for synthesis of a quaternary ammonium compound by a reaction of said mixture with benzyl chloride under stirring and at an elevated temperature. The mass ratio of the tertiary amines-benzyl chloride mixture is between 1.57 and 1.81. It is preferred that the use is made of benzyl chloride refined by distillation at the atmospheric pressure and a temperature of 177-178° C. The derived quaternary ammonium compound consists essentially of dimethyl dodecyl benzyl ammonium chloride and tetradecyl dimethylbenzyl ammonium chloride, the mass ratio of which is controllable. The product can be obtained in the form of gel. Where water or an organic solvent is added to the reaction mixture, a dissolved product is obtained. The product is free from alkyl radicals with the number of carbon atoms over 14, is low-toxic, and its purity is at least 95 mass %. The proposed invention renders it possible to use inexpensive and procurable raw materials, to lower energy intensity and process time, 1 claim, 1 fig., 3 tabl., 5 emb.
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Page/Page column 4
(2008/06/13)
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- 3-NITROISOXAZOLES AND THEIR USE IN THE PROTECTION OF MATERIALS
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The 3-nitroisoxazoles of the formula (I) in which R1 and R2 are each as defined in the description, some of which are known, are highly suitable for use as biocides for protecting industrial materials.
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- O-aryl dithiazole dioxides
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The invention relates to new O-aryldithiazole dioxides, to two processes for their preparation, and to their use as pesticides in crop protection and in the protection of materials.
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- Interactions between biocide cationic agents and bacterial biofilms
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The resistance of bacterial biofilms to physical and chemical agents is attributed in the literature to various interconnected processes. The limitation of mass transfer alters the growth rate, and physiological changes in the bacteria in the film also appear. The present work describes an approach to determination of the mechanisms involved in the resistance of bacteria to quaternary ammonium compounds (benzalkonium chloride) according to the C-chain lengths of those compounds. For Pseudomonas aeruginosa CIP A 22, the level of resistance of the bacteria in the biofilm relative to that of planktonic bacteria increased with the C-chain length. For cells within the biofilm, the exopolysaccharide induced a characteristic increase in surface hydrophilicity. However, this hydrophilicity was eliminated by simple resuspension and washing. The sensitivity to quaternary ammonium compounds was restored to over 90%. Staphylococcus aureus CIP 53 154 had a very high level of resistance when it was in the biofilm form. A characteristic of bacteria from the biofilm was a reduction in the percent hydrophobicity, but the essential point is that this hydrophobicity was retained after the biofilm bacteria were resuspended and washed. The recovery of sensitivity was thus only partial. These results indicate that the factors involved in biofilm resistance to quaternary ammonium compounds vary according to the bacterial modifications induced by the formation of a biofilm. In the case of P. aeruginosa, we have underlined the involvement of the exopolysaccharide and particularly the three-dimensional structure (water channels). In the case of S. aureus, the role of the three-dimensional structure is limited and drastic physiological changes in the biofilm cells are more highly implicated in resistance.
- Campanac,Pineau,Payard,Baziard-Mouysset,Roques
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p. 1469 - 1474
(2007/10/03)
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- Quaternization reaction of some N,N-dimethylalkylamines with benzyl chloride
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The parameters which influence the quaternization reaction of some N,N-dimethylalkylamines of RN(CH3)2, type (R = octyl, decyl, dodecyl, tetradecyl and hexadecyl) with benzyl chloride were studied. By thermogravimetric analyses, the kinetic parameters, the reaction order, "n", and the activation energy, "Ea", of the thermal decomposition of the quaternary salts prepared in this study, were established.
- Avram, Ecaterina
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- Arylthio-dithiazindioxides and their use as pesticides
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PCT No. PCT/EP97/07242 Sec. 371 Date Jun. 23, 1999 Sec. 102(e) Date Jun. 23, 1999 PCT Filed Dec. 22, 1997 PCT Pub. No. WO98/29400 PCT Pub. Date Jul. 9, 1998The invention relates to novel S-aryl-dithiazine dioxides, to processes for their preparation and to the use in crop protection and in the protection of materials.
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- Methods, compositions, and dental delivery systems for the protection of the surfaces of teeth
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The present invention discloses compositions containing lecithin and/or bactericidal compounds, and hydrophobic materials which form, upon application to dental surfaces, adhesive, protective and bacteria-inhibiting barriers.
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- Methods, compositions, and dental delivery systems for the protection of the surfaces of teeth
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The present invention discloses compositions containing a transfer agent and/or bactericidal compounds, and hydrophobic materials which form, upon application to dental surfaces, adhesive, protective and bacteria-inhibiting barriers.
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- Solvatochromism in aqueous micellar solutions: Effects of the molecular structures of solvatochromic probes and cationic surfactants
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Solvatochromic behavior of 2,6-diphenyl-4-(2,4,6-triphenyl-1-pyridinio)- 1-phenolate (RB); 1-methyl-8-oxyquinolinium betaine (QB); sodium 1-methyl-8- oxyquinolinium betaine-5-sulfonate (QBS); and 1-methyl-3-oxypyridinium betaine (PB) was studied spectrophotometrically in micellar solutions of the following cationic surfactants: cetyltrimethylammonium chloride, cetyldimethylbenzylammonium chloride, dodecyltrimethylammonium chloride, and dodecyldimethylbenzylammonium chloride. Microscopic polarity of water at the (average) solubilization site of the solvatochromic probe, E(T) in kcal mol- 1, was calculated from the position of the longest-wavelength absorption band of the probe. The visible spectrum of PB, the most hydrophilic probe, is not affected by surfactants because it is not included in the micellar pseudo phase. For the other three solvatochromic probes, calculated E(T) values depend on the structures of both the probe and the surfactant, namely, its headgroup and long-chain alkyl group. RB, the most hydrophobic probe, samples a much lower microscopic polarity than QB and QBS because it penetrates deeper into the cationic micelle. This conclusion has been confirmed by 1H NMR. Polarities measured by (zwitterionic) QB and (anionic) QBS differ because the latter probe exchanges with the surfactant counterion. Calculated E(T) values refer to micelle-bound probes and are, therefore, different from those reported in the literature, typically determined at [surfactant] ≤ 0.05 mol L-1. Effective water concentrations at the solubilization sites of these solvatochromic probes has been calculated by using as references mixtures of water with each the following organic solvents: n-propanol and dioxane (RB); ethanol, n-propanol, acetonitrile and dioxane (QB and QBS).
- Novaki, Luzia P.,El Seoud, Omar A.
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p. 1957 - 1964
(2007/10/03)
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- Kinetics of the pH-independent hydrolysis of 4-nitrophenyl chloroformate in aqueous micellar solutions: Effects of the charge and structure of the surfactant
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The pH-independent hydrolysis of 4-nitrophenyl chloroformate in the presence of aqueos micelles of sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, alkyltrimethylammonium chlorides, alkyldimethylbenzylammonium chlorides (alkyl group = cetyl and dodecyl) and polyoxyethylene (9) nonylphenyl ether was studied spectrophotometrically. The observed rate constants, kobs, decrease in the following order: cationic micelles > bulk water > non-ionic micelles > anionic micelles. Surfactant-substrate association constants, Ks, were determined from the dependence of kobs on surfactant concentration, and were found to be only slightly dependent on the charge of the surfactant and, for similarly charged micelles, on the length of their hydrophobic tail. A 1H NMR study of the solubilzation of a model compound, 4-nitrophenyl chloroacetate, showed that all surfactant segments are affected by the solubilizate and the effect is more pronounced toward the middle of the hydrocarbon chain. The average solubilization site of the acetate ester does not depend on the charge of the micelle or the length of the surfactant hydrophobic tail. Micellar effects on observed rate constants are analyzed in terms of a 'medium' effect and an 'electrostatic' effect. The lower microscopic polarity at the reaction site retards the reaction, whereas electrostatic interactions of the polar transition state with the charged interface result in a rate decrease by anionic micelles and a rate enhancement by cationic micelles. Copyright
- Possidonio, Shirley,Siviero, Fabio,El Seoud, Omar A.
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p. 325 - 332
(2007/10/03)
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- Method for virus inactivation in the presence of polyalkylene glycol as well as the pharmaceutical preparation obtained therewith
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The invention relates to a pharmaceutical preparation comprising a plasma protein wherein said preparation is free of infectious agents as well as essentially free of denaturation products and is obtainable by a method that encompasses the following steps: a) addition of a polyether and a chaotropic agent to a solution comprising the plasma protein, optional lyophilization of the solution; b) inactivation of infectious agents in the presence of the polyether by a physio-chemical or chemical treatment, and c) removal of the polyether and the chaotropic agent.
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- Termite-controlling agent composition
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Combating termites with a composition comprising (a) at least one compound of the formula STR1 wherein, R denotes a hydrogen atom, acyl, alkyl or optionally substituted heteroarylalkyl, A denotes a hydrogen atom, alkyl or a bivalent group which binds to B, D denotes alkyl, --S--R1, STR2 or bivalent group or atom which binds to A. wherein R1 or R2 each independently denotes a hydrogen atom, acyl, alkyl or optionally substituted heteroarylalkyl. Y denotes =N-- or STR3 wherein T1 denotes a hydrogen atom or optionally substituted alkyl, and X denotes an electron attracting group, and (b) a pyrethoid compound.
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- Agrochemical compositions and methods employing hymexazol and 1,2-benzisothiazolin-3-one
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A combination of 3-hydroxy-5-methylisoxazole with an antimicrobial agent has good agricultural fungicidal activity which lasts longer than 3-hydroxy-5-methylisoxazole alone. The dihydrate of the calcium salt of 3-hydroxy-5-methylisoxazole has advantages over the free 3-hydroxy-5-methylisoxazole, other salts and the anhydrous compound.
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- Bactericidal water-soluble complexes
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Novel bactericidal water-soluble complexes comprising a quaternary ammonium salt and a tricyclic, cage-type heterocycle containing four nitrogen atoms in molar ratios of 1:4 and 3:2 which are effective against both gram negative and gram positive bacteria, fungi, molds, and algae and to a novel method of killing same and novel pesticidal compositions.
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- Pilocarpine salts
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Pilocarpinium 2-naphthalenesulfonate, pilocarpinium 2,5-dihydroxybenzoate, pilocarpinium dihydrogenphosphate, pilocarpinium 2-chloro-4,6-disulfamoylphenoxide, and pilocarpinium 3,5-di-tert-butylsalicylate, novel compounds effective in the treatment of glaucoma.
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- Anticalculus composition
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This invention relates to an improved composition for inhibiting dental plaque and calculus formation, comprising zinc ions and a non-toxic, organoleptically acceptable antibacterial agent in an orally acceptable medium, and to a process for retarding the growth of dental plaque and calculus by application to the teeth of the above composition.
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- Production of unsaturated acids, esters and nitriles, and catalyst therefor
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Alkanoic acids, esters of such acids, and alkyl nitriles are reacted with formaldehyde in the presence of a basic catalyst comprising pyrogenic silica to form α,β-unsaturated acids, the esters of such unsaturated acids or α,β-unsaturated nitriles. The pyrogenic silica is especially effective when treated with activating agents which provide basic sites on the pyrogenic silica catalyst support, such as organic bases, inorganic bases of Groups IIA and IIIA metals, and precursors of such bases.
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