36 results about "Trichloromethyl chloroformate" patented technology

The invention discloses a novel synthesis method of palonosetron hydrochloride, which comprises that (1) (S)-tetralin formic acid is reacted with thionyl chloride and (S)-3-amido-quinine cyclic amine, to obtain (S, S)-quinuclidine tetralin formamide, (2), (S, S)-quinuclidine tetralin formamide is reacted with reductant and boron trifluoride diethyl etherate, to obtain (S, S)-tetralin methyl quinine cyclic amine, (3), (S, S)-tetralin methyl quinine cyclic amine is reacted with diphosgene to be added and reacted in boron trifluoride diethyl etherate solution, while the product is added and reacted with alcaine and water, to obtain palonosetron hydrochloride. And the synthesis route is represented as above: a: SOCI2, (S)-3-aminoquinuclidine, b: NaBH4, BF3OEt2, c: BF3OEt2, CICO2CCI3.

The invention belongs to the technical field of organic compounds and in particular relates to a method for preparing dicyclohexyl methane diisocyanate by a non-phosgene method. In the method, 4,4'-diamino dicyclohexyl methane or an isomer mixture thereof or salt thereof or a mixture of amine and salt thereof, serving as a raw material, reacts with di(trichloromethyl)carbonic ester or trichloromethyl chloroformate or a mixture of the di(trichloromethyl)carbonic ester and the trichloromethyl chloroformate in an inert solvent. By the method, defects of long process route, complex technology, low safety and the like in the preparation of the 4,4'-dicyclohexyl methane diisocyanate by the traditional phosgene method are overcome. The method has the advantages of convenience of operation, high safety and environmental friendliness. In the method, reactants are charged and metered accurately and rate of charge is reduced, so production safety coefficient is improved. Tail gas is simple in treatment; hydrogen chloride gas generated by the reaction is absorbed by water; high-purity hydrochloric acid can be prepared; chloride ions can be utilized completely; and environmental friendliness is contributed.

The invention belongs to the technical field of organic compounds and in particular relates to a method for preparing methylcyclohexyl diisocyanate by non-phosgene. The method comprises the following step of: reacting methylcyclohexyl diamine or an isomer mixture thereof or salt thereof or a mixture of amine and salt thereof as a raw material with bis(trichloromethyl)carbonate or trichloromethyl chloroformate or a mixture of the bis(trichloromethyl)carbonate and the trichloromethyl chloroformate in an inert solvent. In the method, the phosgene is replaced by the bis(trichloromethyl)carbonate or the trichloromethyl chloroformate or the mixture of the bis(trichloromethyl)carbonate and the trichloromethyl chloroformate; and the bis(trichloromethyl)carbonate or the trichloromethyl chloroformate or the mixture of the bis(trichloromethyl)carbonate and the trichloromethyl chloroformate reacts with methylcyclohexyl diamine or salt thereof to prepare the methylcyclohexyl diisocyanate. Compared with the traditional phosgene method, the method provided by the invention has convenience for operation, high safety, environment friendliness and mild reaction condition; and because the charging and the reaction are performed in normal pressure, the requirements on production equipment are reduced, and the process is simplified.

The invention discloses a preparation method of a halogen-free environment-friendly polyurethane oil paint. The preparation method comprises the following steps: performing refluxing catalytic hydrogenation reduction on a phosphatizing agent and a nitrobenzene derivative in an organic solvent with the presence of a metal catalyst to obtain a phosphatized aniline derivative, dropwise adding trichloromethyl chloroformate, mixing and stirring uniformly at room temperature, reacting continuously for 2-4 hours to obtain phosphatized phenyl isocyanate, stirring the phosphatized phenyl isocyanate and an alcoholic compound for 3 hours with the presence of a polymerization catalyst, adding an amine compound, stirring continuously for 2 hours, performing vacuum dewatering on a reaction mixture to obtain flame-retardant polyurethane resin, adding a curing agent and a solvent, and reacting to obtain the halogen-free environment-friendly polyurethane oil paint. The invention further discloses the halogen-free environment-friendly polyurethane oil paint. The halogen-free environment-friendly polyurethane oil paint is an expansive environment-friendly flame-retardant polyurethane oil paint with a phosphorous-nitrogen synergistic effect. In the production process of a flame retardant, raw materials are cheap and easily obtained; the preparation method is free of a high-heat and high-pressure process, and simple to operate, and energy consumption in the production process is low; the whole production process is saves energy and is environment-friendly.

The invention provides a process for synthesizing 4-Nitrobenzyl chloroformate, which comprises reacting trichloromethyl chloroformate or bis(trichloromethyl)carbonate with p-nitrobenzyl alcohol at -40-20 deg C under the action of acid-binding agent, finally carrying out post-treatment to obtain the outcome yield.

The invention discloses a method for synthesizing 2, 6-dichlorobenzoxazole, which takes 2-hydrosulphonyl-6-dichlorobenzoxazole as raw material and trichloromethyl chloroformate or dicarbamate (trichloromethyl) as a chlorinating agent, and the raw material and the chlorinating agent react at the temperature of 65-120 DEG C to prepare the 2, 6-dichlorobenzoxazole; wherein, the mol ratio between the raw material and the chlorinating agent ranges from 1:0.2 to 2. The method has simple technique, safe use and high yield.

The invention discloses a production process of 1, 4-phenylene diisocyanate. The production process includes: heating a solution of p-phenylenediamine and triethylamine to 100 DEG C, adding the heated solution and the chlorobenzene solution of di-(trichloromethyl) carbonate or the chlorobenzene solution of trichloromethyl chlorocarbonate into a reaction kettle, heating until reflux occurs, continuing adding the chlorobenzene solution of di-(trichloromethyl) carbonate or the chlorobenzene solution of trichloromethyl chlorocarbonate, rectifying, and collecting a 130-136 DEG C/8mmHg rectifying product, wherein the reaction kettle comprises a drive motor, a stirring shaft and stirring blades, an automatic sampling device is mounted on the stirring shaft and comprises a sleeve and a sampling component, the sleeve is provided with a liquid storage cavity inside, and the sleeve comprises an annular fixed component located on the upper portion and an annular rotatable component located on the lower portion. The production process has the advantages that the sleeve, the sampling component and the stirring shaft can rotate synchronously by the annular fixed component and the annular rotatable component, real-time sampling during reaction is achieved, and sampling efficiency is increased.

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.

The invention discloses a method for preparing bensulfuron methyl. The method comprises the following steps of: mixing o-methyl formate benzyl sulfamide, bis(trichloromethyl) carbonate and normal-butyl isocyanate serving as a catalyst in dimethylbenzene, heating to the temperature of between 70 and 85 DEG C, heating to the temperature of between 110 and 130 DEG C slowly, adding trichloromethyl chloroformate slowly at the temperature of between 110 and 130 DEG C, performing esterification reaction at the temperature of between 110 and 130 DEG C, and removing a solvent and the catalyst after reaction; and adding o(methyl formate) benzyl sulfonyl isocyanate obtained by the esterification reaction into a condensation reaction solvent, stirring, cooling to the temperature of between 30 and 50 DEG C, continuing to add 2-amino-4,6-dimethoxy pyrimidine, performing condensation reaction at the temperature of between 50 and 90 DEG C, cooling, and drying to obtain the bensulfuron methyl. By the method, the bensulfuron methyl of which the content is more than 97 percent can be obtained, and the total yield is more than 90 percent.

The invention discloses a synthesis process of pyrethroids hapten compound by using dimethyl trichloromethyl chloroformate, gamma-aminobutyric acid and as main material, which comprises following steps that firstly generating 3-(2, 2-dimethyl-3-(2'-methacryloyl) cyclopropyl carbonyl amino) ethyl propionate, secondly generating 3-(3-ethyoxyl-3-oxopropanecarbonic acyl radical)-2, 2-dimethyl cyclopropane aminic acid, thirdly generating 2-hydroxy-2-(3-pheonexyphenyl) acetonitrile, fourthly generating cyano-(3-phenoxy phenyl) methyl N-2-ethyoxylcarbonylethyl-2, 2-dimethylcypromethyl carbonate, fifthly generating 3-(3-(( cyano(3-phenoxyphenyl) methoxyl) carbonic acyl radical)-2, 2-phenoxy phenylcypro carbamoyl) ethylformic acid. Hapten which is prepared by the invention comprises three similarity structures of most pyrethroids pesticides, ester with-CN and three-membered ring structure.

The invention relates to a method for preparing 2, 6-dichlorobenzoxazole, adopting 6-chlorine-2-mercaptobenzoxazole and trichloromethyl chloroformate to synthesize 2, 6-dichlorobenzoxazole under the action of catalyst. The method comprises the following concrete steps that: the 6-chlorine-2-mercaptobenzoxazole, dimethylformamide as catalyst and toluene as medium solvent are added to a reaction vessel with the temperature controlled to be between 40 and 70 DEG C; trichlorome-thylchloroformate is added in drops for 4-8 hours; after drop adding is completed, the materials are heated to between 60 and 100 DEG C, react for 1-4 hours and are cooled, and then a toluene solution of the 2, 6-dichlorobenzoxazole is obtained. The method replaces gaseous phosgene, chlorine or phosphorus pentachloridewith the trichloromethyl chloroformate; during reaction, the trichloromethyl chloroformate is decomposed into single phosgene to participate in the reaction, and then the target object 2, 6-dichlorobenzoxazole is obtained through the reaction. The method does not need to separate the product from the solvent, is simple and convenient to operate, high in product yield, which can reach over 98 percent, pale in product color, excellent in product quality and low in equipment requirements, and does not need tail gas treatment.

The present invention relates to preparation process of trichloro sucrose-6-ester, and is especially preparation process of trichloro sucrose-6-ester with trichloromethyl chloroformate as chlorinating reagent. After trichloromethyl chloroformate is dropped into organic amine solution of sucrose-6-ester at the temperature of -10 deg.c to +20 deg.c, the mixed solution is heated slowly to 80-120 deg.c and reacted for 1-3 hr; and the reacted liquid is further treated through neutralization with alkali solution, decompression stilling to eliminate solvent, dissolving in water, extracting, decolorizing and concentrating to obtain trichloro sucrose-6-ester. Of the material, the weight ratio between sucrose-6-ester and trichloromethyl chloroformate is 1 to 1.5-5. Using trichloromethyl chloroformate with low toxicity as chlorinating reagent results in simple post-treatment, basically no pollution and low cost. The organic amine solvent may be recovered for reuse, and the present invention has high yield.

The invention relates to a method for synthesizing a 2-methyl-2-propyl-1, 3-propanediol diester carbonate compound by using trichloromethyl chloroformate, which comprises the following steps: using 2-methyl-2-propyl 1, 3-propanediol and the trichloromethyl chloroformate as raw materials to completely react with each other under the action of an organic amine catalyst in an organic solvent at a temperature of between 5 DEG C below zero and 50 DEG C, and separating and purifying reaction solution to obtain the 2-methyl-2-propyl-1, 3-propanediol diester carbonate, wherein the molar ratio of the 2-methyl-2-propyl 1, 3-propanediol to the trichloromethyl chloroformate to the organic amine catalyst is 1 to 0.5-2.5 to 0.2-2.5. The method adopts the trichloromethyl chloroformate to prepare the key intermediate 2-methyl-2-propyl-1, 3-propanediol diester carbonate of carisoprodol, has high yield, safety, no pollution, and simple operation and is a synthetic route with broad industrialization prospect.

The invention discloses a synthetic method of a surfactant. The synthetic method comprises the following steps: (1) adding fatty alcohol, a catalyst and amino acid ester into a reactor; (2) closing the reactor, and slowly heating to 200-300 DEG C; (3) carrying out a heat preservation reaction for 2-10 hours; (4) degassing; and (5) treating to obtain a finished product. According to the invention,fatty alcohol is directly selected as an acylation reagent to perform a reaction, so that the step of fatty acid acylation is omitted, the selection of dangerous substance acylation reagents such as phosgene, thionyl chloride, trichloromethyl chloroformate, phosphorus trichloride, phosphorus pentachloride and phosphorus oxychloride is reduced, the emission of byproducts such as phosphorous acid and the like is reduced, and the method is feasible from the aspect of reaction mechanism; and fatty alcohol and amino acid ester are selected to be subjected to a direct reaction, so that impurities such as chlorine ions and the like are not introduced in the process, and the target product is obtained through the direct reaction so as to eliminate the steps of acidification, salification or waterwashing desalination and reduce the use and discharge of salt-containing wastewater or an organic solvent.

The present invention relates to a preparation method of trichloromethyl chloroformate and its special-purpose equipment. It includes the following steps: placing methyl chlorocarbonate in an enamel reactor still; under the double catalytic action of liught and phosphorus pentachloride and under the conditino of that the reactor still temp. is 50-80 deg.C continuously introducing chlorine gas into the reactor still in speed of 8-15 kg/hr. to make chlorination reaction to produce trichloromethyl chloroformate and hydrogen chloride; reaction time is 48-70 hr., detecting specific weight of material d1(35 deg.C)=1.61-1.62, after the reaction reaches to end point, stopping introduction of chlorine gas, cooling and discharging to obtain the invented finished product trichloromethyl chloroformate whose purity is greater than or equal to 98%.

The invention relates to a preparation method of 1-chloroethyl cyclohexyl propyl carbonate and belongs to the field of chemicals. The preparation method of 1-chloroethyl cyclohexyl propyl carbonate comprises the following steps of: adding triethylamine or pyridine or N,N-dimethylaniline into trichloromethyl chloroformate at the temperature between 10 DEG C below zero and 0 DEG C, and dropwise adding paraldehyde to carry out reaction; adding triethylamine or pyridine or N,N-dimethylaniline after reaction, dropwise adding cyclohexanol under the condition that the temperature in a reactor is below 20 DEG C, and stirring to carry out reaction; taking a product of reaction, washing with water, and distilling by reducing pressure to obtain an organic phase which is 1-chloroethyl cyclohexyl propyl carbonate. The synthesized 1-chloroethyl cyclohexyl propyl carbonate is high in yield and purity and low in cost, and the preparation method of 1-chloroethyl cyclohexyl propyl carbonate is easy to control in the preparation process, is easy to operate, is low in risk and is particularly suitable for industrial production.

The present invention is directed to a process for the preparation of Efavirenz, (4S)-6-chloro-4-(cyclopropy-lethynyl)-4-(trifluoromethyl)-1,4-dihydro-2H-3,1-benzoxazin-2-one, of formula (I) comprising reacting the intermediate of formula (II) [0045] as a free base or a salt thereof, with diphosgene (TCMCF, trichlormethylchloroformate) Cl₃CO—COCl in an organic solvent or in a biphasic medium comprised of an organic solvent and water, preferably but not mandatorily in the presence of a weak base in an amount sufficient to neutralise the reaction mixture or in an up to 30% molar excess of such amount.