391 results about "Chloroformate" patented technology

The invention relates to a novel spirodiclofen compound and a preparation method and application thereof. The structure of the novel spirodiclofen compound is shown in a general formula I. The synthesis method of the novel spirodiclofen compound comprises the steps of: in the presence of an acid binding agent, in an aprotic solvent, reacting a compound with a structure formula II with chloro-carbonic ester with a structure formula shown in the description at room temperature, and separating and purifying a product to prepare the novel spirodiclofen compound. The novel spirodiclofen compound can be used for killing pests or mites.

Copolyorganosiloxanecarbonates are prepared by first preparing an oligomeric aromatic polycarbonate, such as an oligomeric bisphenol A polycarbonate, in the presence of a tertiary amine as the only catalyst species; contacting the oligomeric polycarbonate mixture with a polyorganosiloxane bis(aryl)chloroformate, such as the bischloroformate of hydroxy-terminated eugenol polydimethylsiloxane; and introducing phosgene and/or chain termination agent either continuously or in stages. A feature of the process is the presence of dihydroxyaromatic compound in only one charge, at the beginning. The products have excellent physical properties, including transparency.

The invention discloses a copper sulfide ore flotation collector as well as a preparation method and application thereof. The collector is alkoxy carbonyl alkyl dithiocarbamate and has a structural formula as shown in the specification, wherein R1 is carbon chain 1-4 alkyl and R2 is carbon chain 2-4 alkyl. The preparation method comprises the following steps: performing nucleophilic substitution reaction on alkylamine, sodium hydroxide and carbon bisulfide to obtain sodium dithiocarbamate; reacting the sodium dithiocarbamate and alkyl chloroformate to obtain a target collector alkoxy carbonyl alkyl dithiocarbamate. The application refers to application of the copper sulfide ore flotation collector in performing flotation on copper sulfide ore and recycling valuable metal minerals in the copper sulfide ore. The collector is capable of realizing effective separation of the copper sulfide ore and pyrite under an ore pulp environment with the pH value of 6-10, reducing the lime consumption, and further effectively recycling useful metals such as gold, silver and molybdenum. Compared with the existing collector, the collector has the advantages of good selectivity and high useful metal recovery rate.

The invention relates to a detection method and application of a carboxy methyl lysine ingredient in food. The detection method comprises the following steps of: carrying out derivatization by a derivating agent after protein acid in a sample is hydrolyzed; obtaining solution to be detected from the derived solution by solid-phase extraction; carrying out qualitative and quantitative analysis on the carboxy methyl lysine ingredient in the food by adopting a tandem mass spectrometry of isotope dilution ultra-performance liquid chromatography, wherein the derivating agent is 9-fluorenylmethyl chloroformate.

The present invention provides a process for making N-alkoxy(or aryloxy)carbonyl isothiocyanate derivatives by reacting a chloroformate with a thiocyanate, in the presence of an organic solvent and a catalytic amount of a N,N-dialkylarylamine, to produce a N-alkoxy(or aryloxy)carbonyl isothiocyanate intermediate product, wherein the intermediate product is converted to a N-alkoxy(or aryloxy)carbonyl isothiocyanate derivative in high yield and purity.

The invention relates to the field of chemical synthesis and particularly relates to a preparation method of tulathromycin. The method comprises protecting a 2-hydroxyl group of demethyl azithromycin through 4-nitrobenzyl chloroformate, carrying out oxidation and epoxidation on a 4"-hydroxyl group, and carrying out deprotection and 4"-epoxy nucleophilic addition through n-propylamine to obtain tulathromycin. Comprised with the prior art, the preparation method has simple processes, mild conditions and a high yield, is free of palladium-carbon hydrodeprotection and is conducive to industrial production.

The present invention provides a process for making N-alkoxy(or aryloxy)carbonyl isothiocyanate derivatives by reacting a chloroformate with a thiocyanate, in the presence of an aqueous solvent and a catalytic amount of a N,N-dialkylarylamine, to produce a N-alkoxy(or aryloxy)carbonyl isothiocyanate intermediate product, wherein the intermediate product is converted to a N-alkoxy(or aryloxy)carbonyl isothiocyanate derivative in high yield and purity.

The invention provides a method for synthesizing Nexavar. The method comprises the following steps: a, dissolving a compound II and a compound III in an organic solvent inert to the compound III and adding appropriate base; b, performing reaction at a reaction temperature between 40 and 150 DEG C so as to generate a crude Nexavar product; and c, performing conventional post-treatment on the crudeproduct, wherein R is hydrogen, methyl, nitro or chlorine; the nitro is on site 4; the methyl or the chlorine is on site 2, 3 or 4; and the compound III is prepared through the reaction of a compoundIV and phenyl chloroformate or the phenyl chloroformate containing substituents on benzene rings in an organic reaction solvent inert to chloroformate at a temperature between 10 DEG C below zero and50 DEG C. The method has the advantages of applying to the preparation of Nexavar on an industrial scale, meeting standards in pharmaceutical industrial production, improving the purity and environmental compatibility of products and improving operability, safety and yield.

The invention discloses a preparation method of an intermediate 5B and azilsartan 1. The preparation method of the azilsartan 1 comprises the following steps: 1) in a solvent, mixing a compound 2B with hydroxylamine to react to obtain a compound 3B; 2) in a solvent, mixing the compound 3B prepared in the step 1) with chloroformate to react under the action of alkali to obtain a compound 4B; 3) in a solvent, carrying out cyclization reaction on the compound 4B prepared in the step 2) to obtain a compound 5B; and 4) in a solvent, carrying out esterolysis reaction on the compound 5B prepared in the step 3) under the action of alkali to obtain the azilsartan 1, wherein R is a C6-C10 aryl group or C1-C4 straight-chain or branched-chain alkyl group. The preparation method of the azilsartan intermediate 5B is described as the step 3). The preparation method has the advantages of fewer impurities, short reaction time, higher technical yield and higher product purity, and is suitable for industrial production.

The present invention relates to a process for the continuous preparation of polycarbonates or diaryl carbonates by the method of the phase boundary process, in which both the mixing of the organic and aqueous phase and the upstream oligomerization step or aryl chloroformate and/or diaryl carbonate preparation step are effected in a special pump.

The invention relates to fluorine contained miazines compound N-4 position alkyl oxygen carbonyl acidylating method, and its use in composing antineoplastic medicine-capecitabine. The invention has the advantages of avoiding using severe toxicity reagent such as, chloro formate, or phosgene etc, stable and easily gaining raw material, easy industrialization operation etc.

The invention discloses a sulbenicillin sodium preparation method, and belongs to the technical field of medicine. According to the preparation method, alpha-sulfophenylacetic acid reacts with chloroformate to produce a mixed anhydride, 6-APA and an organic alkali are subjected to salt formation, and then dissolved in an organic solvent, the obtained material is subjected to a condensation reaction in the mixed anhydride solution, acidification liquid separation is performed after completing the reaction, the organic phase is retained, and sodium2-ethylhexanoate is added to the organic phase to carry out salt formation to obtain the sulbenicillin sodium, wherein the sulbenicillin sodium is further subjected to sterile crystallization through a system comprising water, ethanol and acetone to obtain sulbenicillin sodium for injection. The preparation method has characteristics of low cost, good quality and easy operation, and is suitable for industrialization.

The invention discloses an active oxygen-responsive polymer support and a preparation method thereof. The preparation method comprises the following steps: mixing 4-(hydroxymethyl) phenylboronic acid pinacol ester with organic alkali and nitrophenyl chloroformate, and stirring to react to obtain NBC; dissolving a water-soluble polymer containing amino into water, adding an organic solvent, so as to form a solution A; dissolving NBC into the organic solvent, so as to obtain a solution B; adding alkali and the solution A into the solution B; stirring to react, and adjusting the pH value of the reaction system to 6.5-7.0, so as to obtain a modified polymer crude product; and purifying crude product, and carrying out freeze-drying, so as to obtain an active oxygen-responsive polymer support pure product. The preparation method of the active oxygen-responsive polymer support is simple, and the prepared arylboronic acid modified polymer support is easy to be chemically coupled with polyphenol active substances containing a catechol structure, so that the water solubility and stability of the support are improved, and the oxygen-responsive release of the support can be realized; and the support has important application prospects in the fields of anti-inflammation, anti-cancer treatment and the like.

The invention discloses an azilsartan intermediate and a preparation method thereof. The preparation method comprises the following step: in a solvent, mixing a compound 3B with chloroformate to react under the action of alkali to obtain a compound 4B. The preparation method has the advantages of fewer impurities, short reaction time, higher technical yield and higher product purity, and is suitable for industrial production.

The invention discloses a trifloxystrobin preparing method, including the steps as follows: (a) using ortho-methyl hypnone as raw material and using potassium permanganate to oxidize so as to obtain 2-(2'-methyl-phenyl)-2-carbonyl acetic acid; (b) making the product in step (a) react with methanol to obtain 2-(2'-methyl-phenyl)-2-carbonyl methyl acetate; (c) bromizing the product in step (b) to obtain 2-(2'-bromomethyl-phenyl)-2-carbonyl methyl acetate; (d) making the product in step (c) react with methoxy amine to obtain (E)-2-(2'-bromomethyl-phenyl)-2-carbonyl methyl acetate-O-methyl ketone oxime; (e) making the product in step (d) react with meta-trifluoromethyl hypnone oxime to obtain the product trifloxystrobin. It reduces the discharge of large amount of waste water in course of oxidization reaction, avoids esterification by adopting methyl- chloroformate, most operating conditions are moderate.

The invention relates to oligoarginine modified phospholipid, nanoparticles assembled by the oligoarginine modified phospholipid, a preparation method of the oligoarginine modified phospholipid and an application of the nanoparticles. After oligoarginine peptide chains are activated by DCC (dicyclohexylcarbodiimide)/NHS (N-hydroxysuccinimide), the oligoarginine peptide chains react with phosphatidyl ethanolamine, purification is performed, and oligoarginine modified phosphatidyl ethanolamine is obtained; or the oligoarginine peptide chains react with DCC/NHS activated phosphatidic acid, and oligoarginine modified phosphatidic acid is obtained through purification; or the oligoarginine peptide chains react with nitrophenyl chloroformate activated phosphatidylcholine, and oligoarginine modified phosphatidylcholine is obtained through purification. The nanoparticles assembled by the oligoarginine modified phospholipid is used for supporting genes, small-interfering RNA, polypeptides or proteinic drugs, antibodies and chemical drugs, and the formed aqueous dispersion of the drug-carrying nanoparticles is used for delivering drugs for in-vitro cells or in-vivo local intravenous injection. The nanoparticles are effectively promoted to enter the cells, and the intracellular drug delivery efficiency is improved.

The invention discloses a method for synthesizing diamide podand extraction agent, wherein chloro-carbonic ester and diglycolic anhydride react to generate mixed anhydride under the action of tertiary amine, and then the reaction is performed with amine to generate the diamide podand extraction agent. The method has mild reaction condition, can be performed at a low temperature, and has high reaction speed and short consumed time; the product purification operation is simple and easy; the obtained diamide podand extraction agent can meet the extraction purity requirement, and is beneficial to establishing flow that the diamide podand is used for treating high-level liquid waste in spent fuel reprocessing plant; the used chloro-carbonic ester is easy to prepare and has a low price, therefore, the cost for preparation of a great amount of extraction agent is greatly reduced; and besides, the yield of the extraction agent is high, so that the method is very suitable for industrial production and application.

The invention relates to a preparation method of 2'3'-di-O-acetyl-5'-desoxy-5-fluoro-N4-(pentyloxycarbonyl)cytidine, belonging to the technical field of medicine. The compound is an important intermediate of Capecitabine. The preparation method comprises the following step: by using anhydrous sodium carbonate or anhydrous potassium carbonate as alkali, quaternary ammonium salt as a phase-transfer catalyst and 4-substituted-pyridine as a catalyst, carrying out amidation reaction on 2'3'-di-O-acetyl-5'-desoxy-5-fluorocytidine and amyl chloroformate to obtain the 2'3'-di-O-acetyl-5'-desoxy-5-fluoro-N4-(pentyloxycarbonyl)cytidine. The invention adopts the anhydrous sodium carbonate or anhydrous potassium carbonate instead of the high-toxicity organic alkali pyridine, and obtains ideal yield and product purity. The method has the advantages of accessible raw materials, low cost, small environmental hazard, high safety and reliability, short reaction time and good product quality.

The invention relates to a preparation process of an ammonia-ester-bond cross-linked poly(ethylene imine) polycation carrier. The preparation process comprises the steps of: adding small-molecular-weight poly(ethylene imine) (PEI), 1,4-butanediol bischloroformate and triethylamine to a reaction solvent, stirring, shaking or vibrating the reaction system to carry out condensation reaction, then dialyzing with a 3500Da reactivated dialysis bag for 48 hours, finally filtering with a 0.22 mu m microporous filtering membrane, and freeze-drying to obtain the product. As compared with the prior art, the preparation process provided by the invention has the advantages that: a purified ammonia-ester poly(ethylene imine) derivative PEI-Bu is prepared; and as compared with poly(ethylene imine) biscarbamate conjugate (PEIC), PEI-Bu displays the highest transfection activity and lower cytotoxicity at a lower mass ratio of PEI-Bu to DNA (deoxyribonucleic acid), is an efficient, low-toxicity gene substance carrier, and can be used for conveying gene substances.

The invention discloses a method for carrying out carbalkoxylation acylation on fluorouracil compound with an active coupling agent, and applications thereof in synthesizing capecitabine. The method comprises the steps of carrying out N-4 site acylation reaction of coupling agent shown as the formula (1) and fluorouracil complex shown as the formula (8), introducing active carbonyl at N-4 site to obtain acylate, directly reacting the acylate with alcohol or phenol without separation, and carrying out N-4 site carbalkoxylation acylation reaction, thus obtaining carbalkoxylation acylate of fluorouracil compound. The carbalkoxylation acylation method can be used for preparing capecitabine. The method conducts acylation and carbalkoxylation acylation on cytidine by adopting coupling agent and alcohol or phenol, thus avoiding use of chlorocarbonic ester or phosgene acylating agent, being used for preparing capecitabine, and being stable and easy to obtain raw materials, high in product purity, safe and environment-friendly for operation environment, and easy for industrial operation.

The invention discloses a preparation method of dabigatran etexilate mesylate, and belongs to the technical field of medicine. The preparation method comprises the following steps: taking 3-[(3-amino-4-methylaminobenzoyl)pyridine-2-ylamino]ethyl propanoate and N-(4-cyanphenyl)amino acetic acid as the raw materials to synthesize an intermediate (S3); making the intermediate (S3) carry out ring-closure reactions to generate an intermediate (S4); subjecting the intermediate (S4) to acid splitting in the presence of a hydrogen chloride-ethanol solution at first, then carrying out ammonification in the presence of ammonia water to generate an intermediate (S5); carrying out reactions between the intermediate (S5) and n-hexyl chloroformate under an alkaline condition to generate an intermediate (S6); dissolving the intermediate (S6), and finally carrying out reactions between the intermediate (S6) and methylsulfonic acid to obtain dabigatran etexilate mesylate. The preparation method has the advantages of simpleness, controllable and mild conditions, high yield, high product purity, stable product property, and suitability for industrial production.