- Hexanoic the trunk decides method for the synthesis of
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The invention discloses a synthetic method of hexamidine. Hexamidine is a key raw material for producing antibiotic medicines hexamidine salts (such as dihydrochloride and dihydroxyethyl sulfonate). The synthetic method of hexamidine comprises the following steps: 1, reacting p-cyanophenol with 1,6-dibromohexane in an ethanol-water solution of sodium hydroxide to prepare 1,6-(p-cyanophenyl)hexyl diether (an intermediate I); 2, carrying out alcoholysis on the intermediate I in ethanol-toluene under the catalysis of trifluoroacetic acid or methanesulfonic acid to prepare 1,6-(p-ethyl iminoformate phenyl)hexyl diether (an intermediate II); and 3, carrying out aminolysis on the intermediate II in a methanol-ammonia solution to prepare hexamidine. The total yield of three-step synthesis is greater than 72%, and a nuclear magnetism identification result shows that the above obtained product is a preconceived structure product. The method is suitable for large-scale industrial production.
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- Preparing method for efficient hexamidine dihydroxyethyl sulfonate
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The invention relates to a preparing method for efficient hexamidine dihydroxyethyl sulfonate. The preparing method is characterized by including the following steps that 1, sodium hydroxide and water are added into an ethanol solution of 4-cyanophenol, after reflux is carried out for 1 h, 1,6-dibromohexane is added, the mixture reacts for 3 h, and the product is filtered and dried to obtain 4,4'-dicyano-1,6-diphenoxy hexane; 2, anhydrous HCl gas is introduced into the product obtained in the previous step and reacts for 72 h at the temperature of 25 DEG C after gas introduction is completed, the product is filtered and dried to obtain 4,4'-imino ethyl ester-1,6-diphenoxy hexane; 3, dry ammonia gas is introduced into the product obtained in the previous step, reaction is carried out at controlled temperature for 15 h, then heating reflux is carried out for 9 h, isethionic acid is added, and a residue is heated to be dissolved, filtered in a suction mode while hot and dried to obtain hexamidine dihydroxyethyl sulfonate. It is found that the reaction has the advantages of being mild in condition, high in conversion rate and short in reaction time and has higher industrialized application value compared with prior synthesis methods.
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