157 results about "Carbonyl chloride" patented technology

The invention belongs to the field of analytical chemistry and particularly relates to an analysis method for simultaneous detection of amino acids and biogenic amines in foods. The method is characterized in that for the first time, 4'-carbonyl chloride-rhodamine is used as a derivatization reagent to realize simultaneous derivatization of the amino acids and the biogenic amines in the food by means of ultrasonic assistance, in-situ derivation and dispersive liquid-liquid microextraction, and qualitative and quantitative detection and analysis are performed by means of ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry in multi-reaction monitoring mode. The method can be used for simultaneous analysis and detection of eight amino acids and nine biogenic amines; by adoption of 1,7-diamino heptane as an internal standard substance, contents of the amino acids and the biogenic amines in different foods can be obtained accurately according to an internal standard method for quantification. The method has advantages of simplicity, quickness, high sensitivity, high selectivity and the like, and high recovery rate is achieved. In addition, by the analysis method, accurate and reliable technical means can be provided for food quality assessment and supervision.

A metal porphyrin lange mull bulogit film optical fiber gas sensor relates to a sensor for checking harmful gas device in industrial condition. The inventive sensor comprises a dual-arm optical fiber, a reaction chamber, and a metal porphyrin LB film array board. The invention is characterized in low check limit, high sensitivity, repeat application, and wide check air range, and the invention can be used to check various volatile harmful gas, more particularly check the discharge and leaked harmful gas as NO2, SO2, NO, CO, H2S and carbonyl chloride.

The present invention relates to a chemical synthesis method of an important intermediate 2-chlorine nicotine acid in medicine and pesticides, and a production process thereof. The route of synthesis reaction comprises: solid carbonyl chloride reacts with N, N-dimethyl formamide, then reacts with ethenyl n-butyl ether, added into dimethylamine aqueous solution, and reacts with cyano ethyl acetate after being dehydrated, the HCl gas is added, and the prepared compound is dissolved in alkaline solution. The raw materials, namely, the solid carbonyl chloride, the N, N-dimethyl formamide, the dimethylamine and the cyano ethyl acetate can be easily acquired. Only one step of distillation and purification is needed from the raw materials to the product; no harsh conditions are required in all the steps, the operation is simple and conducive to the environmental protection, and the present invention has remarkable social benefits and economic benefits, and is suitable for industrial production.

The invention belongs to the field of analytical chemistry and particularly relates to a detecting method for determining various neurotransmitters on the basis of in situ derivation. The method is characterized in that 4'-carbonyl chloride-rhodamine is used as the derivative reagent for the first time, the ultrasonic assistance-in situ derivation-dispersive liquid-liquid microextraction technology is used to derive amino acid and monoamine neurotransmitters, and the ultra-high performance liquid chromatography triple quadrupoles tandem mass spectrum with multiple reaction monitoring modes is used to perform qualitative and quantitative detection; three internal standard substances (isoprenaline, 5-ketoindole-2-carboxylic acid and norleucine) are used for building the linear equations of the neurotransmitters of three chemical structures; the existence of the neurotransmitters is accurately determined by quantification through an internal standard method. The detecting method is simple, fast, high in sensitivity, good in selectivity, good in recovery rate, capable of fast and accurately determining the neurotransmitters, and the like.

The invention relates to a one-pot method for preparing ropivacaine. According to the invention, L-piperidine-2-carbonyl chloride is prepared from L-piperidine-2-carboxylic acid; intermediate separation is not needed, and the material is directly subjected to a reaction with 2,6-dimethylaniline, and (S)-N-(2,6-dimethylphenyl)piperidine-2-carboxamide is prepared; intermediate separation is not needed, and the material is directly subjected to a reaction with bromopropane, such that ropivacaine is prepared. According to the invention, when the intermediate is prepared, no separation is needed, and reactions can be directly carried out. The method is green and environment-friendly. With the method, process operation is simplified, cost is reduced, and yield is improved. The method is more suitable for large-scale industrialized productions.

The invention discloses a method for preparing 3-(3,4-dichlorophenyl)-1-methoxy-1-methyl urea, which comprises the following steps: taking carbonyl chloride as an acylating agent to carry out an acylation reaction with 3,4-dichlorophenyl; obtaining 3,4-dichlorophenyl isocyanate; generating 1-hydroxy-3-(3,4-dichlorophenyl) urea by the reaction of 3,4-dichlorophenyl isocyanate and hydroxylamine sulfate or hydroxylamine hydrochloride under an alkaline condition; neutralizing 1-hydroxy-3-(3,4-dichlorophenyl) urea and alkali; and obtaining 3-(3,4-dichlorophenyl)-1-methoxy-1-methyl urea by a methylation reaction of 1-hydroxy-3-(3,4-dichlorophenyl) urea and dimethyl carbonate under the condition with a catalyst and a solution. The invention has less quantity of three wastes, high yield, good quality and complete reaction, and can reduce pollution and the cost.

A synthesis process of 5-amino-2, 4, 6-triiodoisophthalic acid acyl chloride, which comprises using m-phthalic acid as starting material, preparing 5-amino isophthalic acid through nitration and reduction, preparing 5-amino-2, 4, 6-triiodoisophthalic acid through iodobenzene reaction, using solid carbonyl chloride as acyl chloride agent and addling initiating agent, conducting acyl chloride reaction towards 5-amino-2, 4, 6-triiodoisophthalic acid to prepare 5-amino-2, 4, 6-triiodoisophthalic acid acyl chloride. The 5-amino-2, 4, 6-triiodoisophthalic acid acyl chloride which is prepared by the invention is mainly used to synthesize intermediate compound of ionic contrast agent.

The present invention provides a method for preparing 1,3-dibenzylimidazoline-2-ketone-cis-4,5- dicarboxylic acid, and is characterized by that it utilizes chlorine gas to make fumaric acid produce electrophilic addition reaction to obtain meso-2,3-dichlorosuccinic acid, in the pressence of phase transfer catalyst the meso-2,3-dichlorosuccinic acid and benzylamine are undergone the processes of benzylamination reaction in the solvent so as to synthesize cis-2,3-dibenzylamine succinic acid, the latter and solid carbonyl chloride and undergone the process of phase transfer catalytic ring-closing reaction in the potassium hydroxide solution so as to obtain the invented product. Its total yield rate is up to 74%.

The invention discloses a method for efficiently producing melatonin, relates to the technical field of melatonin synthesis, and aims to solve the problems that purity and an extraction rate of melatonin are relatively low and preparation cost is relatively high in the prior art. According to the method, 5-methoxy indole is taken as 100% of a raw material, carbonyl chloride accounts for 98% of theraw material, ammonium hydroxide accounts for 57% of a generation compound, and lithium aluminum hydride accounts for 80% of the generated compound. The 5-methoxy indole (1) is taken as a raw material, and a carbonyl chloride reaction solvent is added to acylate the 5-methoxy indole, so that a reaction is carried out to generate a compound (2); the generated compound (2) is stranded, and then anammonium hydroxide solvent is mixed with the generated compound (2) according to a certain usage amount to generate a compound (3); and after the compound (3) is generated, a lithium aluminum hydridereagent is added to carry out a reduction reaction on the compound (3) to generate a compound (4).

The invention discloses a preparation method and applications of an oriented immobilized PEGA composite resin. The preparation method comprises following steps: 2-amino-6-chloropurine and 4-nitrobenzyl alcohol are taken as raw materials for Williamson ether synthesis so as to obtain 4-nitryl-O6-benzylguanine; 4-nitryl- O6-benzylguanine is subjected to reduction reaction with protection of t-butyloxycarboryl; coupling reaction of an obtained compound with gamma-aminobutyric acid protected by carbobenzoxy chloride is carried out in the presence of ethyl dimethyl carbodiimide and 1-hydroxybenzotriazole; O<6>-benzylguanine derivative modified PEGA resin is obtained via reduction, separation and purification, reaction with PEGA, and deprotection; and transalkylation reaction of the O<6>-benzylguanine derivative modified PEGA resin with a protein containing MGMT label is carried out, so that oriented immobilization on PEGA resin surface via thioether covalent bonds is realized. Reaction of the preparation method is stable; the steps are simple; a stable uniform protein coating with uniform orientation can be formed on solid material surface by a prepared product; and the preparation method is used for preparing reagent kit with specific recognition effects.

The invention discloses a filgotinib synthetic method and belongs to the technical field of chemical synthesis of medicines. 6-chloro-2-aminopyridine and di-tert-butyl dicarbonate ester are subjected to condensation reaction to obtain 6-chloro-2-tert-butyloxycarbonyl aminopyridine; hydrolysis reaction is performed; the obtained 6-chloro-2-tert-butyloxycarbonyl aminopyridine and trifluorinated methyl sulfonic anhydride are subjected to trifluoromethanesulfonic acid esterification reaction; the obtained 2-tert-butyloxycarbonylamino-6-pyridyltrifluoromethanesulfonate and [(1,1-dioxo-4-thiomorpholinyl)methyl]benzo-4-boronic acid pinacol ester are subjected to condensation reaction to obtain a tert-butyl ester derivative; the tert-butyl ester derivative is treated by trifluoroacetic acid and subjected to de-protection; the obtained intermediate and ethoxycarbonyl isothiocyanate are subjected to isothiocyanate reaction; the obtained intermediate and hydroxylamine hydrochloride are subjected to ring closing reaction; the obtained intermediate and cyclopropane carbonyl chloride are subjected to amidation reaction to obtain the finished product. Operation is simplified; reagents are available; the concept of environment friendliness and environment protection is embodied.

The invention provides octade carbonyl tributyl citrate plasticizer and preparation method thereof. The composition of octade carbonyl tributyl citrate plasticizer (in mass percent): tributyl citrate 43.5-53.8%, octade carbonyl chloride 45.2-55.0%, catalyst 1.0-1.5%. The preparation method comprises: (1) adding citric acid, butylalcohol, water-carrying agent and catalyst into reaction kettle, stirring, heating up until reflowing to obtain tributyl citrate; (2) adding stearic acid into reaction kettle, stirring, heating up to 50 degree and then adding phosphorous trichloride and heating up to 75 degree to perform thermal insulating reaction for 3 hours and layering to obtain octade carbonyl chloride; (3) adding tributyl citrate and catalyst in the reaction kettle, stirring, heating up to 70 degree and then adding octade carbonyl chloride to obtain chlorine hydride and the chlorine hydride being absorbed in water containing soda in drier, when the pH of the water containing soda is constant, the reaction being stopped and the product being subjected to neutralizing, cleaning, pump filtering under reduced pressure to obtain octade carbonyl tributyl citrate.

The invention discloses a recovery method for rhodium from a deactivated catalyst used in formylation of propenyl hydrogen. The method realizes high efficiency recovery of rhodium by directly preparing RhCl(CO)(TPP)2 with a rhodium phosphine complex-containing waste liquid of a catalyst used in formylation of propenyl hydrogen as a starting raw material. The method comprises the following steps: subjecting the catalyst waste liquid to oxidation treatment under an acidic condition so as to break a rhodium cluster; synthesizing rhodium triphenylphosphine carbonyl chloride in a nitrogen atmosphere; and carrying out filtering, washing and drying so as to obtain rhodium. According to the invention, process conditions are mild, equipment used in the method is simple, burning or high temperature treatment is not needed, and little pollution is posed to the environment; the method has the advantages of high yield, simple process and mild conditions, substantially simplifies process flow from catalyst waste liquid to catalyst and reduces treating procedures generating high environmental pollution, e.g., burning, so the method has considerable economic benefits and social benefits.

The invention relates to a method for preparing alpha-alkylated ketone by coupling alcohol with alpha-methyl/methylene ketone. The method comprises the following steps: sequentially adding alpha-methyl/methylene ketone compounds and alcohol compounds into a reaction solvent, then, adding 2mol% of catalyst bistriphenylphosphine rhodium carbonyl chloride (RhCl (CO) (PPh3) 2), finally adding an inorganic alkali, and reacting at 50-100 DEG C to obtain reaction liquid after the reaction is completed; and filtering, concentrating and column chromatography separating the reaction liquid according to a conventional method to obtain the alpha-alkylated ketone. The method provided by the invention is efficient, rapid and environmental-friendly.

A method for synthesizing the 2,4-dichlorobenzoyl chloride belongs to a field of intermediate synthesis of the compound, including catalyzing the 2,4-dichlorobenzotrichloride and carboxylic acid to produce single or compound coarse acyl chloride in the effect of the catalyzer; then rectifying to get corresponding acyl chloride. The advantages of the invention is that environment of the production is clean; the catalyzer can be recycled; carbonyl chloride with low boiling point may be drived off in time so as to get a high empty yield.

The invention relates to the field of optical imaging, in particular to a radix stemonae alkaloid analogue near-infrared fluorescent probe and a preparation method thereof. The near-infrared fluorescent probe is applied to rapid detection of biological mercaptan, and is applied to imaging of the biological mercaptan in cells and living bodies. Existing reported fluorescent probes for detecting thebiological mercaptan have certain limitations, such as complex synthetic routes, long response time, short emission wavelength and the like. The preparation method of the near-infrared fluorescent probe comprises the following steps: 5-(hydroxymethyl)-7-methyl-3, 3 a-dihydrocyclopenta [ b ] chroman cyclo-1 (2H)-one and 3, 7-bis (dimethylamino)-10H-benzothiazine-10-carbonyl chloride react under the action of 4-dimethylamino pyridine and pyridine to generate (7-methyl-1-oxy-1, 2, 3, 3 a-tetrahydrocyclopenta [ b ] chroman cyclo-5-yl)-methyl-3, 7-bis (dimethylamino)-10H-benzothiazine-10-carboxylate.

The invention relates to a photoluminescent room-temperature ionic liquid preparation method. The photoluminescent room-temperature ionic liquid preparation method includes that under an action of thionyl chloride, carboxyl-functionalized naphthaline (pyrene) is converted into naphthyl (pyrenyl) carbonyl chloride, using the naphthyl (pyrenyl) carbonyl chloride to interact with amino imidazole (pyridine) to generate intermediate naphthoyl (pyrene acid) aminoimidazole (pyridylamine); in the presence of triphenylphosphine and carbon tetrabromide, branched alkyl alcohol is converted into branched alkyl halohydrocarbon, and the intermediate naphthoyl (pyrene acid) aminoimidazole (pyridylamine) and the branched alkyl halohydrocarbon are subjected to quaterisation reaction to generate naphthaline-ring-contained (pyrene-ring-contained) photoluminescent room-temperature ionic liquid. The generate naphthaline-ring-contained (pyrene-ring-contained) photoluminescent room-temperature ionic liquid is novel in structure, high in heat stability, low in melting point and adjustable in viscosity and solubility, has photoluminescent characteristics in a solution or in a solvent-free condition and is applicable to the field of fluorescent labels, photoelectric devices and the like.

The invention provides a preparation method of buprofezin, comprising the steps of 1), adding sodium thiocyanate and water into an esterification kettle until dissolution; adding tertiary butanol andhydrochloric acid to obtain a mixed ester; allowing transposition and catalytic reaction to obtain t-butyl isothiocyanate; 2), adding the t-butyl isothiocyanate into chlorobenzene, stirring, dropwiseadding isopropyl amine to obtain 1-isopropyl-3-tert-butylthiourea solution; 3), adding N-methylaniline into chlorobenzene; introducing carbonyl chloride and chlorine gas in sequence to obtain N-chloromethyl-N-benzenecarbamoylchloride solution; 4), adding sodium bicarbonate into water, and adding the resultant into chlorobenzene; adding the 1-isopropyl-3-tert-butylthiourea solution; dropwise addingthe N-chloromethyl-N-benzenecarbamoylchloride solution, filtering, allowing layering, performing high-vacuum steaming to remove the chlorobenzene, crystallizing, centrifuging, and drying to obtain buprofezin. The substitutive average yield of the preparation process of buprofezin reaches 90% and above; the content of finished buprofezin reaches 98.0% and above; the preparation process is free ofammonia nitrogen wastewater.

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 method for preparing di-tert-butyl dicarbonate. The method comprises the steps of: adding sodium tert-butoxide and normal hexane in a reaction kettle, heating until the sodium tert-butoxide and the normal hexane resolve completely under the protection of N2, stirring and cooling to 0 to 50 DEG C; after introducing carbon dioxide into the reaction kettle until satiation, adding a three way catalyst into the liquid reactant; controlling the internal temperature of the reaction kettle to a range from minus 12 DEG C to 20 DEG C; adding solid carbonyl chloride into the reaction kettle for 10 times every 0.5 hour, and reacting for 3 hours after adding is finished; after reacting, adding water and washing, and vaporizing the normal hexane solvent off under normal pressure to obtain a crude product of di-tert-butyl dicarbonate; and crystallizing at the temperature of below 0 DEG C, and centrifugalizing the mother liquid after crystallizing is finished completely so as to obtain the required di-tert-butyl dicarbonate.