13 results about "Glycine ethyl ester" patented technology

The invention belongs to the technical field of cooling agent synthesis, and provides a mint amide cooling agent WS-5 and a preparation method thereof. The method comprises the following steps: mixing menthol, pyridine and acetone, and dropwise adding a chloramine reagent solution to obtain menthone; the preparation method comprises the following steps: mixing a tetrahydrofuran solution of menthone with potassium tert-butoxide, and adding p-toluenesulfonyl methyl isocyanide for reaction to obtain nitrile-based menthol; the method comprises the following steps: dissolving nitrile menthol in hydrochloric acid, and reacting to obtain menthic acid; menthic acid, glycine ethyl ester, pyridine and ethyl acetate are mixed, and a condensation reagent solution is added for reaction. According to the preparation method disclosed by the invention, menthol is oxidized into menthone by using a cheap and easily available chloramine reagent; p-methylbenzenesulfonyl methyl isocyanide is used as a nitrile group source, so that the use of a highly toxic reagent is avoided; according to the method, the menthyl formic acid and the glycine ethyl ester are directly condensed, so that the use of high-pollution reagents is avoided while the reaction steps are simplified, the reaction time is shortened, and the production efficiency is improved.

The invention belongs to the field of organic synthesis, and particularly relates to an efficient method for preparing ethyl chrysanthemate by using a Beta / CuCl nano molecular sieve catalyst. Glycine ethyl ester hydrochloride and sodium nitrite react in a heptane solvent to generate ethyl diazoacetate, and then ethyl diazoacetate reacts with octa-carbene to generate ethyl chrysanthemumate. The catalyst provides an acidic environment and active sites, promotes generation of diazo compounds, controls reactant diffusion through a pore channel structure, and improves the reaction rate and selectivity. The catalyst stabilizes the carbene intermediate and reduces the reaction temperature. The catalyst can be recycled, and environmental pollution and cost are reduced. The yield of the ethyl chrysanthemate exceeds 98%, the yield and quality are improved, and a new scheme is provided for the sanitary insecticide and pharmaceutical industry.

The invention relates to the technical field of preparation of organic compounds, in particular to a spiro [1-benzofuran-3-ketone-2, 3 '-pyrrolidine] compound and a preparation method of the spiro [1-benzofuran-3-ketone-2, 3'-pyrrolidine] compound. According to the method, an aurone compound derived from 1-benzofuran-3-one and imine derived from glycine ethyl ester are used as raw materials, metal salt and alkali react with imine at room temperature to convert into an methylenimine ylide intermediate, and then the methylenimine ylide intermediate and aurone are subjected to [3 + 2] cycloaddition reaction to obtain the spiro [1-benzofuran-3-one-2, 3 '-pyrrolidine] compound. The used reaction raw materials are simple and easy to obtain, the reaction process conditions are mild, post-treatment is simple and convenient, the substrate applicability is wide, and the prepared spiro [1-benzofuran-3-one-2, 3 '-pyrrolidine] compound is high in yield.

The invention discloses a diazotization process for producing ethyl chrysantheate, which is characterized in that the reaction ratio of glycine ethyl ester hydrochloride, water, sodium nitrite, water, glacial acetic acid and toluene is (480 + 660) kg: (262.5 + 660) kg: 36.8 kg: 800L, and comprises the following steps: S1, sequentially adding materials: sequentially adding tap water, glycine ethyl ester hydrochloride, acetic acid, toluene and a sodium nitrite aqueous solution into a diazotization kettle; wherein the sodium nitrite aqueous solution is added dropwise; according to the method, high-precision temperature control is performed on the sodium nitrite aqueous solution, so that the sodium nitrite aqueous solution is prepared efficiently and stably, uniform stirring is performed in a dropwise adding manner, the uniformity and the reaction rate of diazotization reaction are improved, sodium nitrite is dropwise added into acetic acid within a specified control range, the reaction stability of diazo liquid is enhanced, and the yield of the diazo liquid is increased. The cyclization reaction rate is improved.

The application discloses a preparation method of D,L-methionine, which comprises the following steps: mixing glycine ethyl ester hydrochloride, benzaldehyde and a solvent, heating to 40-50 DEG C, opening a negative pressure and a reflux water separation device, keeping the system outside steam by adjusting the negative pressure, and dropping triethylamine; solid-liquid separation is performed on the reaction solution, the liquid is heated to reflux, 2-chloroethyl methyl sulfide is dropped, and reflux reaction is continuously performed; the temperature of the reaction solution is reduced to less than or equal to 60 DEG C, the reflux is stopped, and hydrogen chloride gas is introduced; solid-liquid separation is performed on the reaction solution, the liquid is heated to reflux, hydrochloric acid is dropped, and reflux hydrolysis reaction is performed; the reaction solution is subjected to rotary evaporation, the remaining material is washed and dried to obtain D,L-methionine. The application adopts the mode of amino protection and removal, avoids the use of cyanide and high-temperature and high-pressure reaction, is safe and environment-friendly in the whole process, has high reaction selectivity, has few side reactions, and the by-products and the solvent are easy to separate, so that the cost is further reduced, and the industrialization popularization is facilitated.

The invention discloses a phosphonamide derivative nucleating agent and a preparation method and application thereof. A methoxyphenol compound is oxidized by iodophenyl diacetate and then reacted with an excess of glycine ethyl ester hydrochloride to prepare a methoxyaniline compound, and then the methoxyaniline compound is reacted with phenylphosphonyl dichloride to obtain a phosphonamide derivative nucleating agent. The nucleating agent of the invention is used for preparing a polylactic acid composition, can provide good nucleation efficiency for polylactic acid during the preparation process, and the nucleation effect is very stable. At a low content, the phosphonamide derivative nucleating agent of the application can not only effectively improve the crystallization ability of PLA, but also achieve the flame retardant effect of PLA. The nucleating agent of the application has the potential for application in multiple fields, is easy to realize large-scale production, and can be widely used in the preparation of industrial polylactic acid plastic products.

The invention provides a cooling agent WS-5 production line. The cooling agent WS-5 production line comprises a feeding module, a reaction module and a purification module, the feeding module comprises a raw material tank area, an alkaline water ingredient metering tank, a glycine ethyl ester hydrochloride water ingredient metering tank, a petroleum ether metering tank and a menthyl chloride metering tank; the reaction module comprises a multi-stage continuous reactor and a reaction liquid intermediate tank; the purification module comprises extraction equipment and distillation desolvation equipment, the cooling agent WS-5 production line can be used for continuous production of the cooling agent WS-5, and compared with an existing intermittent production mode, the safety and the production efficiency are greatly improved. Meanwhile, the invention further provides a production process of the cooling agent WS-5.

This invention relates to the field of feed additive preparation technology, and proposes a method for preparing ethyl guanidine hydrochloride, comprising the following steps: S1, dissolving glycine ethyl ester hydrochloride in a solvent, adjusting the pH to 10-11 at 0-5°C using an alkaline adjuster to obtain a reaction solution containing free glycine ethyl ester; S2, adding a cyanamide aqueous solution to the reaction solution containing free glycine ethyl ester at 0-5°C, and reacting at 55-80°C to obtain a reaction solution; S3, after cooling the reaction solution, adjusting the pH to 6-7 using an acidic adjuster, precipitating a solid, which is then filtered and washed to obtain crude ethyl guanidine hydrochloride; S4, recrystallizing the crude ethyl guanidine hydrochloride to obtain ethyl guanidine hydrochloride. This technical solution solves the problems of low yield and low purity of ethyl guanidine hydrochloride in related technologies.

The application discloses a continuous synthesis method of benzylaminoethyl acetate. The continuous flow synthesis method can realize accurate control of reaction conditions, improve the selectivity and purity of products. In addition, the continuous flow synthesis method feeds the reactants at a suitable rate, avoids violent reaction under high concentration, and improves the safety of the production reaction. By designing a continuous flow micro-reaction module, glycine ethyl ester hydrochloride and a catalyst triethylamine are dissolved in toluene under a nitrogen atmosphere to obtain a homogeneous material A; another reactant benzaldehyde is material B. By adjusting the liquid flow meter, the feeding rate of A is adjusted to 36.96 ml / min, and the feeding rate of material B is controlled to 4.41 ml / min by a liquid plunger pump. After material A and material B are continuously synthesized in the micro-reaction module, the products flow into the product storage tank.

The invention discloses a glycine ethyl ester hydrochloride synthesis method, which comprises: (1) adding glycine and absolute ethyl alcohol into a reactor, continuously introducing dry hydrogen chloride, carrying out pre-reaction treatment, and carrying out final reaction treatment; (2) cooling the reaction liquid, and then carrying out centrifugal separation treatment; (3) adding a water removal agent into the reaction mother liquor, carrying out water removal treatment, then carrying out centrifugal separation treatment to obtain a solid, namely the water-absorbed water removal agent, and an obtained filtrate, namely the water-removed mother liquor, and supplementing absolute ethyl alcohol into the water-removed mother liquor for recycling; and (4) carrying out regeneration treatment on the water removal agent after water absorption. According to the novel method for synthesizing glycine ethyl ester hydrochloride, high-temperature backflow is not needed, a water-carrying agent is not introduced, a solvent and water do not need to be separated from mother liquor through rectification, water in the reaction mother liquor is removed through a water removal agent at the room temperature, the mother liquor obtained after water removal can be recycled, and the water removal agent can be regenerated and reused.

The invention discloses a synthetic method of efficient (R)-(2-(4-((6-chlorobenzoxazole-2-yl) oxy) phenoxy) propionyl) glycine ethyl ester. (R)-2-(4-((6-chlorobenzoxazole-2-yl) oxy) phenoxy) propionic acid, methylsulfonyl chloride and glycine ethyl ester hydrochloride are used as raw materials, and high-yield and high-purity (R)-(2-(4-((6-chlorobenzoxazole-2-yl) oxy) phenoxy) propionyl) glycine ethyl ester is obtained by a one-pot method under the catalysis of an acid-binding agent. The method is a one-pot reaction method, has the advantages of simple process, mild reaction conditions, convenience in operation, no need of dangerous reagent thionyl chloride, phosgene and other raw materials, few three wastes, safe and environment-friendly operation process, relatively cheap and easily available raw materials, low reaction cost and suitability for industrial production, and is a green process route.

The present invention relates to the technical field of organic synthesis, and in particular to a synthetic method for 1-amino-2-methyl-2-propanol, comprising the steps of: adding glycine ethyl hydrochloride to an organic solvent, reacting with di-tert-butyl dicarbonate under alkaline conditions to prepare compound compound III; reacting compound III with a Grignard reagent to prepare compound IV; and reacting compound IV with trimethylchlorosilane to prepare 1-amino-2-methyl-2-propanol. The present invention uses cheap glycine ethyl hydrochloride as a raw material, first protects the amino group with Boc, then reacts with a Grignard reagent and an ester to generate a tertiary hydroxyl group. The method is simple to operate, has a high yield, and is suitable for large-scale production.

The invention discloses a method for quantitatively determining the activity of a blood coagulation factor XIII based on fluorescence, which comprises the following steps: (1) treating a plasma sample with bentonite to obtain a plasma sample; (2) adding a plasma sample into the reaction system, and then incubating to obtain a to-be-detected sample; the reaction system comprises a buffer solution, calcium chloride, polyethylene glycol, glycine ethyl ester, himedinium bromide and a fluorescent substrate; (3) establishing a standard curve; and (4) FXIII activity detection: detecting the to-be-detected sample by using the fluorescence tester to obtain the fluorescence intensity of the to-be-detected sample, and calculating the concentration of the to-be-detected sample according to the standard curve. By optimizing the pretreatment process of the plasma sample, the influence of other proteins in the plasma on blood coagulation factor detection is remarkably reduced, and the measurement accuracy is improved.