105 results about "Glycine ethyl ester" patented technology

The invention relates to a preparation method of anagrelide hydrochloride, and relates to preparation methods of chemical raw materials. The preparation method provided by the invention mainly solves the technical problems that an existing synthetic line of anagrelide hydrochloride is long, a toxic reagent, namely cuprous cyanide is used in the synthetic line, many impurities exist in the product, the product is hard to purify and the cost and unit consumption are high. The preparation method comprises the following steps: 1, preparing 2, 3-dichlorbenzyl alcohol; 2, preparing 2, 3-dichloro-6-nitrobenzyl alcohol; 3, preparing 2, 3-dichloro-6-nitryl-benzyl chloride; 4, preparing N-(2, 3-dichloro-6-nitrobenzyl) glycine ethyl ester hydrochloride; 5, preparing N-(6-amino-2, 3-dichlorobenzyl) glycine ethyl ester; 6, preparing an anagrelide hydrochloride crude product; and 7, preparing anagrelide hydrochloride. The preparation method provided by the invention is simple in synthetic process, shorter in synthetic line, low in cost and unit consumption, high in yield and less in three wastes generated in the reaction process, and is suitable for industrialized production. The preparation method provided by the invention is applied to the field of preparation of chemical raw materials.

A method for preparing (S)-oxiracetam comprises the steps of conducting a reaction of a glycine ethyl ester hydrochloride with (S)-4-halogen-3-hydroxy-ethyl butyrate in an alcohol solvent in an alkaline condition, wherein the glycine ethyl ester hydrochloride and the (S)-4-halogen-3-hydroxy-ethyl butyrate are adopted as raw materials, filtering, washing filtrate with inorganic alcohol, concentrating, then extracting, separating and introducing ammonia water to prepare a crude product, and purifying the crude product; and dissociating the glycine ethyl ester hydrochloride into glycine ethyl ester by diethyl ether and ammonia gas firstly. Purification treatment comprises the steps that the crude product of (S)-oxiracetam is dissolved in a benign solvent to prepare a saturated solution, and then the saturated solution is dispersed in a closed environment by a poor solvent. According to the method, the main raw materials are low in cost, easy to obtain and environment-friendly; the glycine ethyl ester hydrochloride is adopted for dissociation, so that the using amount of the materials in the reaction is reduced effectively, the cost is lowered, and in addition, the glycine ethyl ester hydrochloride plays an active role in the reaction yield. The HPLC (high-performance liquid chromatography) purity of the prepared (S)-oxiracetam reaches up to more than 99.0%, the yield is high and reaches up to 36%, the reaction condition is moderate, the operation is simple, and the industrialized scale production is facilitated.

The invention provides a novel method for preparing 3-(3-chloropropyl)-4-oxopyrrolidine-1-ethyl carboxylate, aiming at solving the technical problems of a traditional 3-(3-chloropropyl)-4-oxopyrrolidine-1-ethyl carboxylate synthesis method in the prior art that a flow is complicated, the environmental hazards are great, the safety is low and the yield is low. The technology takes glycine ethyl ester and ethyl acrylate as starting raw materials, and steps of taking benzylamine as a raw material and carrying out debenzylation in a subsequent process are reduced; a process for preparing the 3-(3-chloropropyl)-4-oxopyrrolidine-1-ethyl carboxylate is greatly simplified; an existing technology needs 6-step reaction, and the technology only needs 5-step reaction, so that the operation is simplified and a production period is shortened; the method is applicable to large-scale industrial production. The technology does not take the benzylamine as the starting raw material, and the generation ofa cancer-causing high-hazard substance, i.e., benzyl chloride, is directly stopped from the source; harms to an ecological environment and body health of people are effectively avoided; a reaction process is safe and accords with environmental protection requirements of China better; the total yield is greatly improved and the yield is greater than or equal to 50 percent.

The invention relates to a preparation method of (S)-oxiracetam, which comprises the following steps: reacting raw materials glycine ethyl ester hydrochloride and ethyl (S)-4-halo-hydroxy-butyrate in an alcohol solvent under alkaline conditions, filtering, washing with inorganic alcohol, concentrating, extracting, concentrating the water phase, introducing stronger ammonia water to react to obtain a (S)-oxiracetam crude product, and carrying out purification treatment on the crude product. The glycine ethyl ester hydrochloride is firstly mixed with the alkali and alcohol solvent, and the raw material ethyl (S)-4-halo-hydroxy-butyrate is dropwisely added and the alkali is added in different batches to control the pH value of the reaction at 8-9. The purification treatment comprises the following steps: dissolving the (S)-oxiracetam crude product in a benign solvent to prepare a saturated solution at room temperature, and dispersing with a poor solvent in a closed environment. The HPLC (high performance liquid chromatography) purity of the prepared (S)-oxiracetam is up to 99.0% %, and the yield can be up to 33%; and the method is mild in reaction conditions, simple to operate and beneficial to industrial large-scale production.

The invention discloses a DL-p-methylsulfonylphenyl serine ethyl ester preparation method, which comprises: 1) adding glycine ethyl ester hydrochloride into ethanol, and carrying out heating reflux; 2) dissolving basic cupric carbonate in ammonia water, and adding into the solution obtained in the step 1); 3) adding KOH into the solution obtained in the step 2) to adjust the pH value of the solution, and adding p-methylsulphonyl benzaldehyde, carrying out a reaction; and 4) after the reaction is finished, recovering ethanol in the reacted substance, adding ammonia water into the residue, regulating the pH value, cooling the solution, filtering, washing with ice water, and drying to obtain the p-methylsulfonylphenyl serine ethyl ester. According to the invention, the target product is generated by carrying out a one-step reaction on glycine ethyl ester hydrochloride and p-methylsulphonyl benzaldehyde under the catalysis of basic cupric carbonate and an alkali, wherein the reaction process does not require the use of concentrated sulfuric acid so as to completely avoid the generation of strong acid wastewater, protect and the environment, avoid the possible danger in the sulfuric acid transportation and production process, achieve the safety and easily improve the operation efficiency.

The invention provides an antibacterial anticorrosive pipeline material and a preparation method thereof. The antibacterial anticorrosive pipeline material is prepared by the following steps: (1) mixing titanium dioxide, nano sliver, nano aluminum oxide, dipentaerythritol diphosphite and water to obtain a mixture, and slowly stirring the mixture for 1-2 hours at a temperature of 50-60 DEG C; (2) drying the mixture in a vacuum drying oven after filtering; (3) mixing a dried object with polybutylene, polypropylene, basalt fibers, a polyvinyl acetate emulsion, liquid acrylonitrile butadiene rubber, calcium lignosulphonate, fatty alcohol-polyoxyethylene ether, N-glycine ethyl ester, N-bromo-succinimide, chlorinated paraffin, silicone oil, 1-methyl pentanol and guar gum, and dispersing in a low-speed dispersing machine; and (4) adding the mixture into a twin-screw extruder to carry out extrusion molding. The antibacterial anticorrosive pipeline material has good mechanical property, and has good corrosion resistance and anti-bacterial property.

The invention discloses a fertilizer for promoting growth of a tea leaf and a preparation method of the fertilizer. The fertilizer comprises the following ingredients in parts by weight: 10-15 parts of vinasse, 5-10 parts of rapeseed meal, 5-10 parts of wheat bran, 10-15 parts of animal waste, 10-15 parts of plant straw, 2-7 parts of biological bacteria, 10-20 parts of water, 0.8-1.5 parts of an insecticide, 1-3 parts of microelements, 2-10 parts of kaolin powder, 0.2-0.5 part of vinyl acetate, and 0.01-0.03 part of glycine ethyl ester hydrochloride. The fertilizer has the beneficial effects that the main ingredients of the fertilizer are mainly from the domestic wastes, are easy to degrade in the natural environment, do not pollute the environment, and improve the quality of the tea leaf; and synthesizing the protease by a plant is promoted, the agrochemical residuals are naturally removed, the nutritional element is adsorbed, the nutritional ingredient needed by the tea leaf is complemented, an injurious insect is killed, the soil is improved, the soil hardening is prevented, and the preparation method is simple.

The invention discloses a preparation method for N-benzyl glycine ethyl ester. The method comprises the following steps: dissolving benzylamine in an organic solvent I, then adding 2-halogenated ethyl acetate, alkali and quaternary ammonium salt, and performing reaction to obtain the N-benzyl glycine ethyl ester. The invention also discloses a preparation method for 1-benzyl-3-piperidone hydrochloride. The method comprises the following specific steps: (1) preparing an intermediate IV (N-benzyl glycine ethyl ester); (2) dissolving the intermediate IV in an organic solvent II, then adding 4-halogenated ethyl acetate and alkali, and performing reaction to obtain an intermediate III; (3) performing reaction between the intermediate III and the alkali, reversely regulating a pH value to 6-8, performing concentration under reduced pressure, extracting by using ethyl acetate, performing washing and drying, and then performing concentration under reduced pressure to obtain an intermediate II; (4) performing reaction on the intermediate II and acid, performing rotary evaporation concentration, and adding a crystal solvent for crystallization to obtain a product. The route synthesis steps are short, the process is novel, the intermediates are high in purity, the product yield is high, and the cost is low.