39 results about "Carbobenzoxy 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.

The invention belongs to the technical field of medicines and discloses cytarabine 5'-O-amino-acid ester, pharmaceutically acceptable salts thereof and a preparation method thereof. The preparation method comprises the following steps of: slowly dropping carbobenzoxy chloride into a solution formed by cytarabine, sodium bicarbonate and N,N-dimethylacetylamide, and obtaining a compound A after reacting at room temperature; using the compound A and N-butyloxy formoxyl-amino acid as raw materials; adding a reagent to the solution to carry out an esterification reaction to obtain the cytarabine 5'-O-amino-acid ester; and then adding acid to obtain a finished product. The pharmaceutically acceptable salts comprise hydrochlorides, sulfates, formates, acetates, mesylates, propionates, butyrates, p-toluene sulphonates, phosphates, bisulfates, maleates, lactates, carbonates, bicarbonates, malonates, and salts formed with acidic amino acids, and the like. The invention can obviously improve the membrane permeability of the cytarabine so as to improve the bioavailability of the cytarabine.

The invention relates to an estrogen amino-acid ester compound with antitumor activity as well as a synthetic method thereof, effectively solving the preparation problems of the estrogen amino-acid ester compound with the antitumor activity. The synthetic method comprises the following steps of: dissolving amino acids or small molecule peptides to an aqueous solution of sodium hydroxide or a saturated solution of sodium bicarbonate, dripping carbobenzoxy chloride, making the solution react until the solution is not purple by developing with ninhydrin or carrying out film detection; washing with aether, removing aether, adjusting the pH value of the water phase with hydrochloric acid until milky white solid occurs and extracting with ethyl acetate; washing mixed solution with distilled water and saturated common salt solution, drying with anhydrous magnesium sulfate, carrying out suction filtration, concentrating and purifying; and then, mixing the mixed solution with sterides nucleus and dissolving the mixture to a reaction solvent, adding a condensing agent and a catalyst, supplementing an additional condensing agent, carrying out film detection, filtering, concentrating and purifying, dissolving in a dissolving solvent, adding palladium carbon for catalytic hydrogenation, detecting the film, filtering, concentrating and purifying. The estrogen amino-acid ester compound withantitumor activity, provided by the invention, has favorable water solubility and is superior to 2-methoxyestradiol in the tumor cell resistance action.

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 novel near infrared ratio fluorescence probe for detecting hydrogen peroxide as well as a preparation method and an application of the probe. The probe is 2-[2-[2-[[4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyloxycarbonyl]benzylamino]-3-[(1,3-dihydro-1,3,3-trimethyl-2H-indol-2-ylidene)ethylidene]-1-cyclohexen-1-yl]ethenyl]-1,3,3-trimethylindolium iodide. The preparation method comprises steps as follows: 1,2,3,3-tetramethyl-3H-iodoindole and 2-chloro-1-formyl-3-hydroxymethylcyclohexene are subjected to a dehydration condensation reaction; obtained 2-[2-[2-chloro-3-[(1,3-dihydro-1,3,3-trimethyl-2H-indol-2-ylidene)ethylidene]-1-cyclohexen-1-yl]ethenyl]-1,3,3-trimethylindolium iodide and benzylamine react; obtained 2-[2-[2-benzylamino-3-[(1,3-dihydro-1,3,3-trimethyl-2H-indol-2-ylidene)ethylidene]-1-cyclohexen-1-yl]ethenyl]-1,3,3-trimethylindolium iodide and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)carbobenzoxy chloride react, and the novel fluorescence probe is obtained. The probe shows higher selectivity for detection of hydrogen peroxide.

The invention relates to a synthetic method of N-fluorenylmethoxycarbonyl-N- triphenylmethyl-D-glutamine to solve the current problems of the shortage of D-Gln raw materials and high cost of synthesizing products from the D-Gln. The synthesis includes the following steps: a. D-glutamate and a carbobenzoxy chloride are reacted to get the N-carbobenzoxy-D-glutamate; in an organic solvent N and N-dimethylformamide with the existence of a triethylamine and bromomethyl-benzene, the N-carbobenzoxy-D-glutamate selectively protects an Alpha-carboxyl to get an N-benzyloxycarbonyl-D-benzyl L-glutamate; b. the triethylamine, ethyl chloroformate and ammonia are added to N- benzyloxycarbonyl-D- benzyl L-glutamate organic solvent with a molar ratio of 1:1:2 to 6; after reacted for 6 to 24 hours under a temperature of -20 to 20 DEG C, an N- benzyloxycarbonyl-D-glutaminebenzylester is gotten; c. the product of b, acetate liquor is reacted with a triphenylmethanol under a catalysis of concentrated sulfuric acid, and N- benzyloxycarbonyl-N-triphenylmethyl-D-glutaminebenzylester can be gotten after reacted for 8 to 24 hours under a temperature of 40 to 60 DEG C; d. benzyloxycarbonyl and benzyl are detracted from the product of c to get the N-triphenylmethyl-D-glutamine; e. the product of d is protected by an Fmoc group to get the N-fluorenylmethoxycarbonyl-N-triphenylmethyl-D- glutamine.

This invention relates to a polyimide-polybenzoxazole precursor solution, a polyimide-polybenzoxazole film, and a method of manufacturing the same, wherein a film manufactured using the polyimide-polybenzoxazole precursor solution of the invention is formed by copolymerizing a unit structure of diamine and dianhydride and a unit structure of diaminophenol and dicarbonyl chloride in an organic solvent, and is colorless and transparent, like conventional polyimide films, and can exhibit improved heat resistance and low birefringence.

The invention discloses a preparation method of tert-butyl N-carbobenzoxy-3-amino-alanine tert-butyl ester, and mainly solves the technical problem of low total yield and high cost in the original process. The preparation method comprises the following steps of 1, suspending asparagine into a mixed solution of water and acetone; regulating the pH value to a basic state by a sodium carbonate solution; lowering the temperature; adding carbobenzoxy chloride; then, raising the temperature for reaction; after the reaction is finished, performing acidification by hydrochloric acid; separating out solid; performing filtering to obtain an intermediate N-benzoxycarbonyl asparagine; 2, suspending the N-benzoxycarbonyl asparagine into dichloromethane; introducing isobutene; adding concentrated sulfuric acid; performing sealed reaction for two days; performing treatment to obtain N-carbobenzoxy asparagine tert-butyl ester; 3, dissolving the N-carbobenzoxy asparagine tert-butyl ester into water andN,N-dimethylformamide; adding iodobenzene diacetate for reaction first; then adding pyridine; continuously performing reaction till the completion; performing treatment to obtain a final product.

The present invention discloses recyclable polymeric catalyst of Formula I, for chlorination of organic acids and alcohols using chlorinating agents such as carbonyl chloride, oxalyl chloride or thionyl chloride,

wherein, ‘m’ on the pendent groups on polystyrene backbone can have values from 1 to 5 and R is the alkyl group ranging from C1 to C5.

The invention relates to a method for preparing polycarbonate. The method utilizes an interface method, and comprises the steps of: mixing alkaline aqueous solution of one or more dihydroxy aromatic hydrocarbons and organic solution of carbonyl chloride(phosgene); controlling the pH value to be between 9 and 12.5 in the whole process; and performing an interfacial polymerization reaction of a phenol chain terminator, the dihydroxy aromatic hydrocarbons and the phosgene in the presence of a catalyst, namely an amphiphilic block copolymer to prepare the polycarbonate. The method utilizes the amphiphilic block copolymer as the catalyst for preparing the polycarbonate by the interface method, which can increase the utilization rate of the carbonyl chloride, reduce the consumption of the carbonyl chloride, and improve the utilization rate of bisphenol; the catalyst can promote the rapid transformation of chloroformate and obtain a polycarbonate product with low inclusion amount of dihydroxy aromatic compounds; and no phenol precipitations are precipitated after a wastewater phase is acidified, and a catalyst material can be treated and recovered by adopting a conventional method.

The invention belongs to the field of medicinal chemistry and particularly relates to an alcaftadine intermediate and a synthetic method for alcaftadine. The method comprises the following steps: taking (1H-imidazo-5-yl)methanol (as shown in a formula II) as a raw material, and producing a hydroxyl protection reaction, a substitution reaction with beta-phenylethyl bromide, an electrophilic substitution with 1-methylpiperidine-4-carbonyl chloride hydrochloride, a cyclization reaction and an oxidation reaction to synthesize alcaftadine (as shown in a formula I). The method provided by the invention does not relate to an imidazole ring hydroxymethylation reaction, and hydroxymethyl in the alcaftadine structure is introduced from a starting material, so that the use of high-temperature condition and a toxic reagent, namely formaldehyde is reduced, the production of bis(hydroxymethyl) byproducts in a hydroxymethylation process is avoided, and the cost is reduced. The alcaftadine intermediate is low in production cost, good in product quality and suitable for industrialized production, and the synthetic raw materials are low in price and easily available.

The invention discloses a polylactic acid copolymer with high glass-transition temperature and a preparation method thereof. Lactide and copolymerization monomer as main raw materials are subjected to ring opening polymerization and polycondensation reactions in the presence of a catalyst, so as to prepare the polylactic acid copolymer. The copolymer contains an aromatic diacid monomer unit and a diol monomer unit with ring structure, has weight average molecular weight of 3-300000 and the glass-transition temperature of 110-200 DEG C. The preparation method of the invention is simple, the raw material is lactide rather than a lactic acid solution, and the aromatic dicarboxylic acid rather than non phosgene or oxalic acid is used. By adjusting the ratio of materials for ring opening polymerization, can be simple, polylactic acid copolymers with different monomer unit ratio can be precisely designed, and the prepared polylactic acid copolymer has high molecular weight and glass transition temperature up to 200 DEG C.

The invention discloses a purification method of an isocyanate silane coupling agent and the isocyanate silane coupling agent, alkyl carbonyl chloride or alkyl sulfonyl chloride is added into a crudeproduct containing the isocyanate silane coupling agent in a nitrogen atmosphere, after full mixing, vacuum distillation is carried out, and the isocyanate silane coupling agent is obtained. The method disclosed by the invention has the beneficial effects that the method is suitable for purifying the isocyanate silane coupling agent prepared by adopting a thermal cracking method, the raw materialsare cheap and easy to obtain, the addition amount is small, the process is simple, the manufacturing cost is hardly increased, and side reactions such as bulk polymerization and the like generated when the isocyanate silane coupling agent is rectified and heated can be effectively inhibited.

The invention discloses a synthesis process of di-tert-butyl dicarbonate. According to the synthesis process, tert-butyl alcohol alkali metal salt and a carbonyl chloride compound are used as reactionraw materials; supercritical carbon dioxide is used as a reaction raw material and a solvent; and synthesis of the di-tert-butyl dicarbonate is carried out in a carbon dioxide supercritical state; the problem that no proper solvent exists in each step of reaction for producing di-tert-butyl dicarbonate is thoroughly solved by utilizing the super-strong solubility and permeability of the supercritical carbon dioxide, the carbon dioxide is used as both the reaction raw material and reaction solvent, so that the reaction is easier, the reaction temperature is increased to room temperature or above, and no side reaction exists; the supercritical carbon dioxide has different solubilities for a product and a by-product, so that the product is directly separated from the by-product, and the problems of post-treatment water pollution and product loss are avoided.

The invention relates to a synthesis method of racemic-(3aR,7aR)-5-(t-butyloxycarboryl)-octahydro furan [3,2-c] pyridine-3a-carboxylic acid. The method mainly solves the technical problem that no proper industrial synthesis method exists in the prior art. The method comprises seven steps that: firstly, 2-bromoethanol and ethyl propiolate react in a solvent of methylene dichloride at the room temperature to obtain a compound 2; then, the compound 2 and ethyl cyanoacetate react in a solvent of N, N-dimethyl formamide at the room temperature over the night to obtain a compound 3; the compound 3 is subjected to catalytic hydrogenation to reduce the cyano groups to obtain amino groups; meanwhile, the exchange with the self ester is performed to obtain a compound 4; a compound 5 is obtained through carbobenzoxy chloride on the compound 4; the compound 5 is reduced by borane to obtain a compound 6; finally, the compound 6 uses a palladium hydroxide as a catalyst in ethanol; meanwhile, Boc estolide is added; hydrogen gas is introduced for overnight reaction to obtain a target compound 7; the compound 7 is hydrolyzed by water and lithium hydroxide in a mixed solution of methanol and water; a final target compound 8 is obtained.

The invention discloses a synthesis method of combined buprofezin, relates to the technical field of synthesis methods of buprofezin, and aims to solve the problem that carbonyl chloride crop organic intermediates are usually used for reaction in the existing synthesis process of combined buprofezin, but carbonyl chloride is a violent suffocating poison gas and can cause harm to human bodies after being inhaled by people. The synthesis method comprises the following steps of: adding N-methylaniline and formic acid into a reaction kettle to prepare N-methyl formyl amine, adding the prepared N-methyl formyl amine, carbon tetrachloride and benzoyl peroxide into a distillation kettle, then introducing chlorine gas to prepare an N-chloromethyl-N-phenyl carbamoyl chloride solution, then preparing tert-butyl isothiocyanate preparing an N-tert-butyl-N'-isopropyl thiourea solution, and adding the prepared N-chloromethyl-N-phenyl carbamoyl chloride solution, tert-butyl isothiocyanate, acetone, dimethyl formamide and potassium hydroxide into a reaction kettle for reaction to obtain buprofezin crystals.

The invention relates to a hypoxic/ROS (reactive oxygen species) responsive prodrug for deeply penetrating and blocking pancreatic duct adenocarcinoma innervation and a preparation method of the prodrug. The preparation method comprises the following steps: (1) reacting N-alpha-fluorenylmethoxycarbonyl-N-epsilon-t-butyloxycarbonyl-L-lysine with 5-amino-1, 3, 4-thiadiazole-2-sulfonamide to obtain (A); reacting (A) with piperidine to obtain (B); (2) dimethyl dithiopropionic acid methane and thionyl chloride are subjected to a reaction, and (C) is obtained; reacting the compound (C) with camptothecin to obtain a compound (D); (3) azobenzene-4, 4-dicarbonyl chloride and lalotinib are subjected to a reaction, and (E) is obtained; (4) reacting maleimide polyethylene glycol with azobenzene-4, 4-dicarbonyl chloride to obtain (F); (F) reacts with (B) to obtain (G); reacting (G) with trifluoroacetic acid to obtain (H); the reaction product (H) sequentially reacts with N6-carbobenzoxy-L-lysine cyclic anhydride and N5-t-butyloxycarboryl-L-ornithine cyclic anhydride, and (I) is obtained; reacting (I) with trifluoroacetic acid, adding (D), and reacting to obtain (J); reacting (J) with hydrobromic acid and acetic acid, adding (F) and iRGD, and reacting to obtain a polymer prodrug (K); the invention also discloses a method for preparing a nano-drug from the polymer prodrug.

The invention discloses a method for the preparation of thiophene-2-carbonyl chlorides starting from thiophenes with oxalyl chloride at elevated temperature with short reaction time.

The invention discloses a mesosulfuron-methyl preparation method, which comprises the following steps: reacting pyrilamine with a carbonyl chloride compound to obtain isocyanate, and condensing the isocyanate with 5-methylsulfonylaminomethyl-2-methoxycarbonyl benzenesulfonamide to obtain mesosulfuron-methyl. The method disclosed by the invention is high in yield, the prepared product is high in purity, and byproducts generated in the preparation process are few and are easy to recover.

The invention discloses a biomass-based slow-release pesticide and a preparation method thereof. The method comprises the following steps: (1) carrying out a first contact reaction on a biomass raw material, fatty alcohol and a first acidic catalyst, and separating the product obtained after the first contact reaction so as to obtain light oil and alcoholysis residue; and (2) carrying out a third contact reaction on the alcoholysis residue and a pesticide drug compound and an optional cross-linking agent in an organic solvent at the pH value of 7-9 and at 30-50 DEG C for 0.5-1 h. The fatty alcohol is C4-C13 aliphatic saturated monohydric alcohol. The cross-linking agent is one or more ingredients selected from a group consisting of carbonyl chloride, thionyl chloride, isocyanate, maleic anhydride and phthalic anhydride. Drug loading capacity of the prepared biomass-based slow-release pesticide reaches up to 25.47 wt%. The pesticide has high insect poisoning efficiency. After three months of the use, the highest inhibition rate of fruit fly eggs still reaches up to 80% and above.