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

The preparation method of organic compound tetrabutyl carbamide uses dibutylamine and trichloromethyl carbonate as raw material, and makes synthesis is organic solvent to obtain the invented product. Said method is safe, has no production of three wastes, its raw materials are non-toxic, its reaction yield is high and quality is good.

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 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%.

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 a medical raw material 7beta-amino-7lapha-methoxy-3-cephem compound. Methods in prior arts have the problems of more steps and low yield. According to the 7beta-amino-7lapha-methoxy-3-cephem compound preparation method provided by the invention, a beta-lactam compound is adopted as a raw material, and is subjected to a reaction with bis(trichloromethyl)carbonate under the existence of an organic alkali, such that a iminochloride-beta-lactam compound is produced; methanol is added for alcoholysis, such that the 7beta-amino-7lapha-methoxy-3-cephem compound is produced. The method provided by the invention has the advantages of mild and easy-to-control reaction conditions, high yield, no product of 7alpha-methoxy-7beta-amino-3-cephem compound isomer, and easy separation. With the method, the 7beta-amino-7lapha-methoxy-3-cephem compound product with ultrahigh purity can be obtained.

The synthesis method for thiazolopyridinone in organic chemical field comprises: using bitrichloromethyl carbonate and o-aminohydroxypyridine with mole ratio of 0.3-0.7 as materials; the thedichloromethane, dichloroethane, trichloromethane, tetrachloromethane, chlorobenzene, benzene, toluene, xylene, and THF as solvent by weight ratio with former carbonate as 1-10; the pyridine, DMF, and triethylamine as initiator by mole ratio with the carbonate as 0.001-1; the pyridine, DMF, triethylamine, hydroxide or carbonate or bicarbonate of alkali metal or alkaline-earth metal as bound acid agent by mole ratio with the carbonate as 6-10; then, stirring to react for 0.5-5h at 0-100Deg. This invention has high yield and product purity with low cost.

A process for preparation of 10-oxo-10,11-dihydro-5H-dibenz[b,f]azepine-5-carboxamide (oxcarbazepine) via intermediate 10-methoxy-5H-dibenz[b,f]azepine-5-carbonyl chloride, comprising the steps: a) Preparation of an intermediate 10-methoxy-5H-dibenz[b,f]azepine-5 carbonyl, chloride from 10-methoxyiminostillbene using bis (trichloromethyl) carbonate (BTC) with organic base such as aliphatic or aromatic tertiary amines in organic solvent; b) Conversion of the intermediate to 10-methoxy-5H-dibenz[b,f]azepine-5-carboxamide using ammonia in organic solvent; c) Formation of oxcarbazepine from step (b) using Bronsted acid in an organic solvent at a temperature between 25° C.-80° C., preferably at 50° C. to 70° C.; and d) Isolation of oxcarbazepine.

The invention discloses a 5-methyl-1, 3, 4-oxadiazole-2 (3H)-ketone and making method, which is characterized by the following: looping acetydrazide and trichloromethyl chloroformate or di (trichloromethyl) carbonate to obtain the product; adopting pyridine or 4-dimethylamino pyridine as catalyst; using 1, 2-dichloroethane as dielectric solvent.

3-(2-chlorophenyl)-5-methyl-4-isoxazole formyl chloride is a key intermediate body of cloxacillin. It uses bis (trichloromethyl) carbonate and makes it directly be reacted with 3-(2-chlorophenyl)-5-methyl-4-isoxazole formic acid instead of sulfur oxycchloride or phosphorus oxychloride or phosphorus pentachloride or phosphorus trichloride or phosgene or diphosgene to synthesize 3-(2-chlorophenyl)-5-methyl-4-isoxazole formyl chloride.

The invention discloses a preparation method of 3-[[[2-[[4-cyanophenyl) amino] methyl]-1-methyl-1H-benzimidazole-5-yl] carbonyl] (pyridine-2-yl) amino] ethyl propionate. The preparation method is characterized by comprising reaction steps as follows: a first reaction of [(4-cyanophenyl) amino] acetic acid and bis(trichloromethyl) carbonate, and then a reaction of 3-[(3-amino-4-methylamino benzoyl) (pyridine-2-yl) amino] ethyl propionate and a product of the first reaction. The preparation method is simple, easy to operation and low-cost.

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 invention discloses a method for synthesizing 2-normal-butyl-4- chloro-5-formylimidazole shown by a formula (I). Imidazolone shown in the formula (II) reacts with bis (trichloromethyl) carbonate shown by a formula (III) and formamide shown by a formula (IV) in an organic solvent for 1-10 hours at the temperature of 20 DEG C below zero to 200 DEG C, and reaction solution is hydrolyzed to obtain 2-normal-butyl-4-chloro-5-formylimidazole. The invention has mild reaction conditions, good selectivity, no generation of phosphorus wastewater and low cost of proposal of waste water, waste gases and waste residues, and is suitable for industrial production.

The invention discloses a cyclic utilization method of production mother liquor in a production method of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride in CN10147982A. The method comprises the stepsof: carrying out heating reflux treatment on production mother liquor to decompose a small amount of residual bis (trichloromethyl) carbonate, carrying out distillation separation treatment to obtaina distillate and a residual solution, recycling the distillate in the production process of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride, and recycling the residual solution in the crystallization process of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride. According to the cyclic utilization method, high-added-value comprehensive utilization of all effective components in the production mother liquor is achieved, production and product performance of 4-ethyl-2, 3-dioxopiperazine-1-formyl chloride cannot be affected, the yield of the target product can be increased to 88.0% or above, and the purity can reach 97.0% or above.

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 relates to synthesis of an important intermediate, namely 2-amino-5-bromo-3-hydroxypyridine, of an anti-tumor drug Lorlatinib (PF-06463922). 2-amino-3-hydroxy pyridine is used as a starting raw material, and subjected tothree steps of reactions including ring closing, bromination and hydrolysis to finally prepare 2-amino-5-bromo-3-hydroxypyridine, wherein in the ring closing step, bis(trichloromethyl) carbonate (BTC) and N,N'-carbonyl diimidazole (CDI) are combined for use; in the bromination step, 2-hydroxy-2-methyl-1-phenyl-1-acetone is used as a photoinitiator, and liquid bromine is used as a brominating agent. Compared with the prior art, the method is more environment-friendly and economical.

The invention relates to a method for preparing 2,4-dihydroxy benzaldehyde. The method comprises the following steps: by taking m-dihydroxybenzene as a raw material, performing reaction on bis(trichloromethyl) carbonate triphosgene BTC and N,N-dimethylformamide DMF in an organic solvent, and purifying, thereby obtaining a target compound. According to the method, as the triphosgene is adopted to replace a phosphorus-containing or sulfur-containing chlorination agent, the problems of treatment of a great amount of phosphorus-containing or sulfur-containing byproducts, discharging of wastewater and the like in the production process are solved, and the method has the characteristics of being easy in raw material obtaining, gentle in reaction condition, simple in operation step, low in cost, low in energy consumption, small in pollution, possible in clean production and the like and has industrial application prospects.

The invention discloses a preparation method of (S)-3-N,N-disubstituted amino-1-(2-thienyl)-1-propanol shown as the formula (I). The method comprises: taking 2-acetyl thiophene shown in the formula (II) as a raw material, and allowing 2-acetyl thiophene to completely react with di(trichloromethyl)carbonic ester (III) and N,N-disubstituted methanamide (IV) in an organic solvent under the catalysis of an organic base to obtain N,N-disubstituted amino-1-(2-thienyl)-1-acrylketone shown as the formula (V); and performing hydrogenation reduction with lithium aluminium hydride to obtain N,N-disubstituted amino-1-(2-thienyl)-1-propanol shown as the formula (VI); and performing splitting with S-mandelic acid and recrystallization with ethyl acetate to obtain the target product shown as the formula (I). The preparation method is low in cost, mild in reaction condition, less in waste water, waste gas and industrial residue, small in energy consumption, and high in yield. The preparation method is safe and is suitable for industrial production.

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 provides a preparation method of a red direct blending dye. The method comprises the following steps: a step of obtaining the scarlet acid: enabling a J acid salt solution to react with bis (trichloromethyl) carbonate to obtain a scarlet acid reaction product, and obtaining the dissolved scarlet acid in the scarlet acid reaction product; the method comprises the following steps: obtaining diazonium salt A: carrying out diazotization reaction on aniline to obtain the diazonium salt A; a step of obtaining diazonium salt B: carrying out diazotization reaction on p-aminoacetanilide to obtain the diazonium salt B; coupling reaction: carrying out coupling reaction on the dissolved scarlet acid, the diazonium salt A and the diazonium salt B to obtain a coupling product; and a post-treatment step: carrying out post-treatment on the coupling product to obtain the red direct blending dye. The red direct blending dye is high in strength and excellent in dyeing performance, almost no waste water is generated in the preparation process, environmental pollution is smaller, and the red direct blending dye has a great promotion effect on clean production.

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 relates to a method for preparing 2, 4, 5-trichloropyrimidine. The method comprises the following steps that: 1) uracil reacts with sodium hypochlorite under an acidic condition to form 5-chlorouracil; and 2) the 5-chlorouracil and bis (trichloromethyl) carbonate react to form 2, 4, 5-trichlorouracil. The preparation method is high in yield and low in cost, has the advantages of being easy to operate, little in pollution, safe, environmentally friendly and the like, and is suitable for large-scale industrial production. The reaction equation is shown in the specification.