39 results about "Bis(trichloromethyl) carbonate" patented technology

The invention relates to an industrial production method for producing clindamycin or the salts of clindamycin. The method uses dual-trichloromethyl carbonate or trichloromethyl methyl chloroformate and amide to prepare the intermediate chlorophthalic agent. The method of the invention has high product purity, high yield, easier post-processing and other technical advantages, compared with the prior art.

The invention discloses a method for synthesizing 3,3',4,4'-benzophenonetetracarboxylic dianhydride by taking o-xylene and bis(trichloromethyl) carbonate as raw materials. The method comprises the steps of: by taking o-xylene and bis(trichloromethyl) carbonate as the raw materials, performing acylation reaction in catalysis of anhydrous lewis acid, thus obtaining bis(3,4-ditolyl)methanone; fully oxidizing bis(3,4-ditolyl)methanone in a potassium permanganate / hydrochloric acid system, and carrying out filtration, concentration, crystallization and the like to obtain 3,3',4,4'-benzophenonetetracarboxylic acid; performing vacuum high-temperature melting and dehydration to 3,3',4,4'-benzophenonetetracarboxylic acid to obtain the 3,3',4,4'-benzophenonetetracarboxylic dianhydride product. The preparation method has the advantages of being simple in technology, high in yield, fewer in three wastes, capable of recycling anhydrous lewis acid, low in production cost and easy for industrial implementation, and the like.

The invention relates to a preparation method of 2-chloro-3-formyl quinoline derivatives. The preparation method comprises the following steps: by taking acetanilide or substituted acetanilide as a raw material, reacting with bis(trichloromethyl) carbonate (BTC) and N,N-dimethylformamide (DMF) in an organic solvent to obtain a target compound. The preparation method provided by the invention has the advantages that bis(trichloromethyl) carbonate is adopted for replacing a phosphorus-containing or sulfur-containing chlorination reagent, so that the problems of treatment of phosphorus-containing or sulfur-containing byproducts and wastewater discharge in a production process are solved, the preparation method has the characteristics that raw materials are easily available, the cost is low, operation steps are simple, reaction conditions are mild, the energy consumption is low, the reaction process is safe, the environmental pollution is small and the clean production can be realized, and the preparation method has industrialization application prospect.

A process for chemically synthesizing symmetrical diarylketone compound includes reaction between aromatic compound and bis-trichloromethyl carbonate in organic solvent under the action of yttarbium trifluoromethane sulfonate, filtering, separating filtered cake, and purifying.

The present invention relates to a chemical synthesis method of 3-phenyl-5-methyl-4-isoxazole formyl chloride. It is made up by using bis (trichloromethyl) carbonate and 3-phenyl-5-methyl-4-isoxazole formic acid as raw material and making them undergo the acyl-chlorination reaction in organic solvent. The product is a key intermediate body of oxazocilline, and said synthesis method is reasonable in technological process, high in reaction yield and low in production cost.

The chemical synthesis method of 3-phenyl-5-methyl-4-isoxazolecarboxylic acid chloride, using bis (trichloromethyl) carbonate and 3-phenyl-5-methyl-4-isoxazolecarboxylic acid as The raw material is prepared by acyl chloride reaction in organic solvent, and the product is the key intermediate of oxacillin. The synthesis method is a chemical synthesis method of 3-phenyl-5-methyl-4-isoxazolecarbonyl chloride with reasonable process, safe and reliable production, high reaction yield, low production cost and basically no three wastes.

The invention discloses concrete with performance improved by using a BTC (bis-trichloromethyl carbonate) functional admixture. The concrete comprises the following components in parts by mass: 200-320 parts of cement, 60-90 parts of mineral powder, 40-60 parts of fly ash, 680-780 parts of sand, 1060-1100 parts of broken stones, 3.3-4.74 parts of a concrete admixture, 1.92-2.58 parts of the BTC functional admixture and 170 parts of water. The BTC functional admixture can improve the cohesiveness of the concrete, reduce the bleeding and segregability of the concrete and enhance the fluidity of the concrete, so that the service life of a pump pipe is prolonged, the use of a cementing material in the concrete is reduced, the cost of the concrete is lowered, the workability of the concrete is improved, and the concrete is convenient to construct.

The invention discloses a synthetic method of emtricitabine intermediates, namely, (2R, 5S)-5-(5'-fluoro-cytimidine-1-group)-1, 3-oxathiolane-2-carboxylic acid-L-menthyl ester having the structural formula of (VI), (2R, 5S)-5-hydroxy-1, 3-oxathiolane-2-carboxylic acid-L-menthyl ester having the structural formula of (III) is taken as raw material to obtain chloro compounds having the structural formula of (IV) by chlorination reaction, then the chloro compounds (IV) are treated with condensation and hydrolyzation reactions with N, O-bis(trimethoxy)5-flurocytosin having the structural formula of (V), thus obtaining the (2R, 5S)-5-(5'-fluoro-cytimidine-1-group)-1, 3-oxathiolane-2-carboxylic acid-L-menthyl ester (VI). The invention uses bis(trichloromethyl) carbonic ester to replace the thionyl chloride in the prior art so as to be taken as a chlorination reagent, thus having the advantages of safe and reliable operation and environmental protection.

The invention relates to the technical field of addition type carbonate flame retardants and provides a method for preparing a phenoxy tetrabromobisphenol A carbonate flame retardant. The method comprises the following steps: (1) dissolving phenol and tetrabromobisphenol A in a chloralkane solution, and uniformly stirring; (2) dissolving bi(trichloromethyl) carbonate in the chloralkane solution in a reaction container at room temperature; (3) adding a catalyst into the reaction container; (4) dropwise adding alkaline liquor and a mixture dissolving solution prepared in the step (1) into the reaction container at a constant speed, and reacting for 1-2 hours at room temperature; (5) washing the solution prepared in the step (4) until the solution does not contain chloridion, and splitting the organic layer; and (6) dropwise adding the organic layer into hot water at the temperature of 70-95 DEG C, and separating out the coarse product by crystallization. According to the method, the target product, namely phenoxy tetrabromobisphenol A carbonate is directly obtained, the molecular weight controllability of the product is improved, the operation process is simple, and the operability is high.

The invention discloses a method for preparing tetrabutylurea by using an oil-water two-phase reaction system, which is characterized in that bis (trichloromethyl) carbonate and dibutylamine are used as raw materials, the oil-water two-phase reaction system is designed and provided, a solvent capable of effectively dissolving bis (trichloromethyl) carbonate and dibutylamine is adopted, meanwhile, a water phase is added into the reaction system to perform liquid seal on the reaction system, can absorb hydrogen chloride gas generated by the reaction at the same time, and promotes the forward proceeding of the whole reaction, and the method has the characteristics of high conversion rate, high selectivity and the like. The method for preparing tetrabutylurea by using the oil-water two-phase reaction system comprises the following steps: dissolving bis (trichloromethyl) carbonate in an organic solvent, placing the solution in a reactor, and simultaneously adding water into the reactor to perform liquid seal on the reaction system; and dissolving dibutylamine in an organic solvent, slowly injecting the dibutylamine into the organic solution of bis (trichloromethyl) carbonate through a micro-injection pump, carrying out chemical reaction, and carrying out refining treatment to obtain the product tetrabutylurea.

The invention discloses a lamivudine intermediate, that is, (2R,5S)-5-(5-cytosine-1-yl)-1,3-oxothioheterocycle with the structure shown in formula (VI) The synthetic method of pentane-2-carboxylic acid-L-menthyl ester is based on (2R, 5S)-5-hydroxyl-1,3-oxathiolane-2 as shown in formula (III) -Carboxylic acid-L-menthyl ester is raw material, obtains structure as the chlorinated product shown in formula (IV) by chlorination reaction, chlorinated product (IV) and structure as shown in the N of formula (V), O-bis( Trimethylsilyl) 5-cytosine condensation, hydrolysis in the system. The present invention uses bis(trichloromethyl)carbonate instead of thionyl chloride in the prior art as the chlorination reagent, and has the advantages of safe and reliable operation, and environmental protection.

The invention relates to the field of chemically synthesized drug, in particular to a new synthetic process of drug for preventing and curing poultry coccidiosis, i.e., toltrazuirl. The synthetic process includes allowing trifluoromethylthiophenol and 2-chloro-5-nitrotoluene as raw material to condense, performing the reduction reaction with hydrogen in presence of Pd / C catalyst, reacting with bis (trichloromethyl) carbonate for esterifying isocyanic acid, and finally adding diethyl carbonate and methylurea for synthesizing toltrazuirl. The new synthetic process of toltrazuirl has easy operation, simple required equipment, low pollution, easily the prior raw material, low cost, and high yield with a total one of up to about 50%.

A method for synthesizing oxazopyridone compounds relates to the field of chemical synthesis, in particular to the field of organic chemical synthesis. The method uses bistrichloromethyl carbonate and o-aminohydroxypyridine as raw materials, and the molar ratio is 0.3 to 0.7; dichloromethane, dichloroethane, chloroform, tetrachloromethane, chlorobenzene, benzene, toluene , xylene, tetrahydrofuran are solvents, and the weight ratio of solvent and bis-trichloromethyl carbonate is 1 to 10; with pyridine, dimethylformamide, triethylamine as initiator, initiator and bis-trichloromethyl carbonate The molar ratio of the ester is 0.001~1; pyridine, dimethylformamide, triethylamine, alkali metal or alkaline earth metal hydroxide or its carbonate or its bicarbonate are used as the acid-binding agent, and the acid-binding agent and The molar ratio of the bis-trichloromethyl carbonate is 6-12; at a temperature of 0-100° C., the oxazopyridone compound is obtained by stirring and reacting for 0.5-5 hours. The invention has the advantages of easy-to-obtain raw materials, safe storage and production process, simple and convenient operation, high yield, high product purity, simple post-treatment and the like.

The invention discloses a green preparation method of 2-chloro-3-cyanopyridine, comprising the following steps: taking 3-cyanopyridine N-oxide as a raw material, dissolving it in a certain amount of organic solvent, adding additives , organic base and phase transfer catalyst to form a raw material system, control the appropriate temperature, then dissolve bis(trichloromethyl)carbonate in a certain amount of organic solvent, and slowly add it dropwise to the raw material system for reaction. Simple processing can give 2-chloro-3-cyanopyridine. The preparation method of the invention is simple, the reaction period is short, and the phosphorus-containing reagent is replaced by green chlorination reagent without heavy metal participation. Compared with the prior art, the invention has less environmental pollution, safe operation, low cost and is suitable for industrialized production. This method is applied to the green chlorination reaction of 3-cyanopyridine N-oxide, but not limited to the preparation of 2-chloro-3-cyanopyridine.

The invention relates to the technical field of addition type carbonate flame retardants and provides a method for preparing a phenoxy tetrabromobisphenol A carbonate flame retardant. The method comprises the following steps: (1) dissolving phenol and tetrabromobisphenol A in a chloralkane solution, and uniformly stirring; (2) dissolving bi(trichloromethyl) carbonate in the chloralkane solution in a reaction container at room temperature; (3) adding a catalyst into the reaction container; (4) dropwise adding alkaline liquor and a mixture dissolving solution prepared in the step (1) into the reaction container at a constant speed, and reacting for 1-2 hours at room temperature; (5) washing the solution prepared in the step (4) until the solution does not contain chloridion, and splitting the organic layer; and (6) dropwise adding the organic layer into hot water at the temperature of 70-95 DEG C, and separating out the coarse product by crystallization. According to the method, the target product, namely phenoxy tetrabromobisphenol A carbonate is directly obtained, the molecular weight controllability of the product is improved, the operation process is simple, and the operability is high.

The invention discloses a preparation method of 4-chloro-7H-pyrrolo[2,3-d] pyrimidine. The preparation method comprises the following steps: enabling 4-hydroxy-7H-pyrrolo[2,3-d] pyrimidine to undergochlorination reaction with bis(trichloromethyl)carbonate (BTC) in a nonpolar organic solvent under the catalysis of organic base; cooling a reaction solution and then adjusting a pH value to 8 to 9; carrying out insulated stirring, suction filtration, water washing and vacuum drying to obtain the 4-chloro-7H-pyrrolo[2,3-d] pyrimidine. According to the preparation method, the BTC is used for replacing phosphorus oxychloride; after the reaction is finished, reduced pressure distillation on the phosphorus oxychloride is avoided, and a large amount of phosphorus-containing wastewater is prevented;by adopting the organic base as a catalyst, the reaction temperature is reduced, and generation of dimolecular impurities is avoided. The method has the advantages of simple operation, greenness, environment friendliness, easiness in industrial production and the like.