A kind of synthetic method of cyanide antidote

Abstract

The invention relates to a cyanide antidote synthesis method, which comprises: adding a formaldehyde solution and p-nitroanisole in an ethanol solution, adjusting the pH value to 4 with hydrochloric acid, heating, slowly adding iron powder, carrying out a reaction after the adding to obtain 4-dimethylaminoanisole, adding the 4-dimethylaminoanisole to toluene, adding aluminum trichloride, carryingout heating reflux, removing the methyl, cooling, adding a saturated sodium bicarbonate solution, filtering out the solid while hot, separating the liquid, carrying out water washing on the toluene phase, separating the liquid, carrying out pressure reducing evaporation to remove the toluene, and carrying out heating evaporation to obtain the product. According to the present invention, the product obtained through the curing has the purity of more than 99% and the yield of more than 80%; and the method has advantages of cheap and easily-available raw materials, no dangerous operation, less wastewater generation, low environmental pollution and high overall yield, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical synthesis, and in particular relates to a synthesis method of a cyanide antidote. Background technique [0002] 4-Dimethylaminophenol is an aromatic compound containing phenol and amine groups, the chemical formula is C 8 h 11 NO, 4-dimethylaminophenol is an antidote for cyanide poisoning. It detoxifies through the production of methaemoglobin, but this is only suitable for acute poisoning, followed by treatment with sodium thiosulfate or cobalamin, In animal experiments, it works by intramuscular injection. [0003] The method that prior art produces 4-dimethylaminophenol has three kinds: [0004] Method 1: The synthetic route is as follows [0005] [0006] This method has a large number of literature reports, and the synthesis method is to add formaldehyde and sodium borohydride in an alcohol solvent, and use sodium borohydride to generate hydrogen, which is risky in production, a...

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Problems solved by technology

[0012] The raw material 4-dimethylaminoanisole of this method is mainly made by reacting p-aminoanisole with dimethyl sulfate or methyl iodide under alkaline conditions, and the reaction yield is low, only about 50%. Both methyl ester and methyl iodide have strong carcinogenic effects, which bring great risks to production. There are mainly two methods in the literature reports for the synthesis of 4-dimethylaminophenol. The first is boron tribromide, which is expensive , which greatly increases the production cost; the second method is to use the hydrobromic acid solution of acetic acid to reflux at 110 degrees Celsius to obtain the product. This reaction produces a large amount of waste acid water, which has a certain pressure on environmental protection

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