38 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 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 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 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 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 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 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.