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33 results about "Ethyl nicotinate" patented technology

Method for synthesizing 2-chloro-3-amino-4-methylpyridine by ethyl cyanoacetate and acetone

The invention relates to a method for synthesizing an important intermediate 2-chloro-3-amino-4-methylpyridine for an anti-AIDS medicament Nevirapine, and belongs to the technical field of organic synthesis. The method comprises the following process steps that: ethyl cyanoacetate and acetone are dehydrated and condensed to generate a condensation compound I under the action of a catalyst; dimethyl formamide, dimethyl sulfate and sodium methoxide solution react to generate N,N-dimethylformamiade dimethyl acetal (N,N-dimethyl formamide A), and then the N,N-dimethylformamiade dimethyl acetal reacts with the condensation compound I to generate conjugated enamine, namely a condensation compound II; the condensation compound II is cyclized by hydrochloric acid and ethanol to form a cyclic compound 2-chloro-4-methyl-ethyl nicotinate; the 2-chloro-4-methyl-ethyl nicotinate is ammonolyzed by ammonia gas to form 2-chloro-4-methyl-niacinamide; and the 2-chloro-4-methyl-niacinamide is subjected to Hofmann degradation reaction to form the 2-chloro-3-amino-4-methylpyridine. Compared with the prior synthesizing method, the method of the invention has the remarkable characteristic of reducing the reaction steps, and is suitable for large-scale industrialized production; the molar total yield of the five-step reaction is improved to 27 percent from the prior 24 percent; and the purity of the product reaches over 99 percent.
Owner:江苏鼎昊医药科技有限公司

Synthesis method of nicotinoyl hydrazone Schiff base compound as well as application of compound to bactericide

InactiveCN108840823AEasy to separateThe synthesis reaction is easy to operateBiocideOrganic chemistryOrganic synthesisFiltration
The invention relates to a synthesis method of a nicotinoyl hydrazone Schiff base compound as well as application of the compound to bactericide, and relates to the technical field of organic synthesis. The synthesis method of the nicotinoyl hydrazone Schiff base compound comprises two steps of synthesizing an intermediate nicotinoylhydrazine and synthesizing a target product, wherein the nicotinoylhydrazine is prepared by carrying out a refluxing stirring reaction among raw materials such as hydrazine hydrate, ethyl nicotinate and absolute ethanol, carrying out a reaction under the conditionof 80 DEG C for synthesis, and performing aftertreatment; the target product is prepared by performing refluxing stirring reaction on the prepared intermediate nicotinoylhydrazine as well as a small amount of glacial acetic acid and aldehyde compound under the condition of 65 DEG C, performing suction filtration and performing recrystallization. The synthesis reaction is simple to operate and theyield of products is high; furthermore, the synthesis method is low in equipment requirement, low in production cost and easy in industrialized large-scale application. In addition, the synthesized nicotinoyl hydrazone Schiff base compound can serve as the bactericide to selectively kill germs, and the prevention effect on wheat powdery mildew can reach to 83.1 percent.
Owner:HUAIHUA UNIV

Preparation method of high-purity L-nicotine medical intermediate

The invention discloses a preparation method of a high-purity L-nicotine medical intermediate, which comprises the following steps: synthesis of myosmin: pumping dry xylene into a condensation reaction kettle, adding metal sodium and tert-butyl alcohol, heating, preserving heat, and cooling for later use; the method comprises the following steps: pumping xylene, ethyl nicotinate and N-vinylpyrrolidone into a reaction kettle, carrying out heat preservation, carrying out stirring until the solution is clear, and pumping the solution into a high position; dropwise adding the high-order reaction liquid into a condensation reaction kettle, heating after dropwise adding, and cooling for later use; adding concentrated hydrochloric acid and water into an acidolysis kettle, stirring and cooling, transferring a reaction solution in the condensation reaction kettle into the acidolysis kettle, transferring a layered lower water layer into a reflux kettle for reflux, transferring into a desolventizing kettle, transferring a desolventizing kettle bottom solution into a myosmin distillation kettle, and distilling off myosmin under reduced pressure; and preparing the L-nicotine. By adopting the preparation method of the high-purity L-nicotine medical intermediate, the high-purity L-nicotine is obtained, the consumption of acid, alkali and organic matters is reduced, and the cost is greatly reduced.
Owner:仙居两山生物科技有限公司

Preparation method of ethyl nicotinate

The invention relates to a preparation method of ethyl nicotinate. The preparation method is characterized by comprising the following steps of: adding nicotinic acid, absolute ethyl alcohol and an esterification reaction solid acid catalyst into methylbenzene; stirring the mixture to react for 3-6h at 50-65 DEG C; then raising the temperature to return and divide water; finishing the reaction till no water is divided; reducing the temperature to room temperature; filtering and recovering the esterification reaction solid acid catalyst; recovering methylbenzene at a reduced pressure from the filtrate; recovering the methylbenzene to obtain a light yellow transparent liquid which is the finished product ethyl nicotinate, wherein the molar ratio of nicotinic acid and absolute ethyl alcohol is 1: 1 to 1: 2; the weight ratio of nicotinic acid and methylbenzene is 1:0.3 to 1:8; the adding amount of the esterification reaction solid acid catalyst is 0.01-0.1 time of the weight of the nicotinic acid; the esterification reaction solid acid catalyst is an HND230 solid catalyst. The preparation method provided by the invention has the advantages of reducing generation of highly polluted wastewater, reducing the manual and equipment costs and being relatively suitable for industrial production on a large scale.
Owner:常州沃腾化工科技有限公司

Method for synthesizing 2-chloro-3-amino-4-methylpyridine by ethyl cyanoacetate and acetone

The invention relates to a method for synthesizing an important intermediate 2-chloro-3-amino-4-methylpyridine for an anti-AIDS medicament Nevirapine, and belongs to the technical field of organic synthesis. The method comprises the following process steps that: ethyl cyanoacetate and acetone are dehydrated and condensed to generate a condensation compound I under the action of a catalyst; dimethyl formamide, dimethyl sulfate and sodium methoxide solution react to generate N,N-dimethylformamiade dimethyl acetal (N,N-dimethyl formamide A), and then the N,N-dimethylformamiade dimethyl acetal reacts with the condensation compound I to generate conjugated enamine, namely a condensation compound II; the condensation compound II is cyclized by hydrochloric acid and ethanol to form a cyclic compound 2-chloro-4-methyl-ethyl nicotinate; the 2-chloro-4-methyl-ethyl nicotinate is ammonolyzed by ammonia gas to form 2-chloro-4-methyl-niacinamide; and the 2-chloro-4-methyl-niacinamide is subjected to Hofmann degradation reaction to form the 2-chloro-3-amino-4-methylpyridine. Compared with the prior synthesizing method, the method of the invention has the remarkable characteristic of reducing thereaction steps, and is suitable for large-scale industrialized production; the molar total yield of the five-step reaction is improved to 27 percent from the prior 24 percent; and the purity of the product reaches over 99 percent.
Owner:江苏鼎昊医药科技有限公司
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