95078-12-9Relevant articles and documents
Benzalkonium chloride preparation method
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Paragraph 0069-0070, (2019/04/26)
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.
Synthetic method of aryl sulphobetaine in solvent-free system
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Paragraph 0028; 0029; 0045; 0046, (2017/04/03)
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.
A synthetic method of a benzalkonium chloride mixture
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Paragraph 0016; 0021; 0022, (2017/08/30)
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.
