41 results about "Oxidative decarboxylation" patented technology

The invention relates to a method for synthesizing an asymmetric diaryl selenide compound. The method comprises the following steps: taking aryl carboxylic acid and diaryl diselenides as reaction materials under oxygen conditions in an organic solvent, and carrying out an oxidative decarboxylation coupling reaction under the combined promotion action of a copper catalyst, a ligand and alkali, thereby obtaining the asymmetric diaryl selenide compound. The method is cheap and highly available in aryl carboxylic acid substrate and copper catalyst, wide in substrate range, simple in reaction conditions and high in product yield and purity, develops a novel synthetic route and method for the asymmetric diaryl selenide compound and has excellent application potential and research value.

The invention belongs to the technical field of chemical products, and relates to a method for improving the fermentation yield of long-chain dicarboxylic acid. According to the method, the long-chain dicarboxylic acid is produced by a microbiological fermentation method by taking C10 to C18 n-alkanes as raw materials; the method is characterized in that alpha oxidative decarboxylation inhibitor and beta-oxidation inhibitor are added in a fermentation production process to reduce the alpha-oxidative decarboxylation and beta-oxidation capacities of strains, wherein the alpha oxidative decarboxylation inhibitor is one or mixture of more of chlorpromazine hydrochloride, phenobarbital sodium, crylic acid and polyacrylic acid, and the concentration is 0.01 to 1mmol / L; and the beta-oxidation inhibitor is one or mixture of more of mercaptoacetic acid, sodium thioglycollate, ranolazine, ranolazine dihydrochloride and mildronate, and the concentration is 0.01 to 1 mmol / L. Compared with the prior art, the method has the advantages of high acid producing speed, weak alpha oxidative decarboxylation and beta-oxidation capacity, low unit consumption of alkane, and high fermentation alkane conversion rate, and is particularly suitable for preparing the long-chain dicarboxylic acid.

The invention provides a novel preparation method of an insensitive explosive TATB. The method comprises the following steps: 1, with 2,4,6-trinitrotoluene as a raw material, subjecting 2,4,6-trinitrotoluene to reacting with hydrogen and acetic anhydride in sequence to obtain 2,4,6-triacetylaminotoluene; 2, subjecting the obtained 2,4,6-triacetylaminotoluene o oxidation and a decarboxylation reaction to obtain 1,3,5-triacetylaminobenzene; and 3, carrying out nitrification and hydrolysis reactions on the obtained 1,3,5-triacetylaminobenzene to obtain 2,4,6-trinitro-1,3,5-triaminobenzene. According to the invention, the raw material used in the preparation method is the cheap 2,4,6-trinitrotoluene, and used reactants or catalysts are commonly used products in the chemical industry, so the preparation method has characteristics of low cost and usage of simple and easily available raw materials. In addition, the preparation method also has the characteristics of short synthesis steps, simple operation of each step, high yield, high reaction rate, easy separation and collection of intermediate and final products and the like, and is beneficial for realization of mass production of TATB.

The invention discloses a synthetic method of 3, 4-methylene dioxybenzaldehyde and relates to the field of chemical organic synthesis, and particularly relates to a synthetic method in which an intermediate generated in a process of preparing 3, 4-methylene dioxybenzaldehyde by taking catechol methylene ether as a raw material is oxidized by suing a nitryl-free oxidizing agent to generate the final product. According to the synthetic method of 3, 4-methylene dioxybenzaldehyde, oxidative decarboxylation is carried out on the intermediate piperonyl mandelic acid (prepared from catechol methylene ether) as an initial reactant in the presence of at least one catalyst selected from metal chloride Lewis acid and at least one oxidizing agent selected from oxygen and peroxides in an acidic environment so as to synthesize 3, 4-methylene dioxybenzaldehyde. The synthetic method provided by the invention is simple in technical step, thorough in conversion of the raw materials, high in finished product yield and short in technical time, and the product does not contain color-changing impurities and is stable in technical quality.

The invention discloses a synthetic method of 3, 4-methylene dioxybenzaldehyde and relates to the field of chemical organic synthesis, and particularly relates to a synthetic method in which an intermediate generated in a process of preparing 3, 4-methylene dioxybenzaldehyde by taking catechol methylene ether as a raw material is oxidized by suing a nitryl-free oxidizing agent to generate the final product. According to the synthetic method of 3, 4-methylene dioxybenzaldehyde, oxidative decarboxylation is carried out on the intermediate piperonyl mandelic acid (prepared from catechol methylene ether) as an initial reactant in the presence of at least one catalyst selected from metal chloride Lewis acid and at least one oxidizing agent selected from oxygen and peroxides in an acidic environment so as to synthesize 3, 4-methylene dioxybenzaldehyde. The synthetic method provided by the invention is simple in technical step, thorough in conversion of the raw materials, high in finished product yield and short in technical time, and the product does not contain color-changing impurities and is stable in technical quality.

The invention relates to a preparation method of 4-acetyloxy-2-azetidinone compounds, and is used for solving the problem that the large-scale industrial production cannot be favorably realized because of defects such as severe reaction condition, complex treatment process, high cost, serious environment pollution and the like in the prior art. The method provided by the invention comprises the step of carrying out oxidization deacidification in the existence of a dehydrating agent N, N'-dicyclohexylcarbodiimide and an oxidizing agent peroxyacetic acid by taking 4-carboxyl-2-azetidinone compounds I as raw materials to obtain the 4-acetyloxy-2-azetidinone compounds II. A heavy metal oxidizing agent or catalyst is prevented from being used in the oxidization deacidification process, so that the residue and discharge of heavy metals and environmental pollution caused by the heavy metals are greatly reduced. Byproducts generated in a reaction process can be conveniently recycled, so that the production cost is reduced to the great extent, and the preparation method is more excellent on the aspect of economical efficiency. The method is mild in reaction condition, simple and convenient to operate and suitable for large-scale production; the 4-acetyloxy-2-azetidinone compounds are easy to separate and purify and high in yield.

The invention provides a preparation method of insensitive explosive TATB. The method comprises: step 1: using 2,4,6-trinitrotoluene as a raw material, successively reacting with hydrogen and acetic anhydride to obtain 2,4,6-triacetamidotoluene; step 2: converting the obtained 2,4 ,6-triacetamidotoluene is oxidized and decarboxylated to obtain 1,3,5-triacetamidobenzene; step 3: the resulting 1,3,5-triacetamidobenzene is nitrated and hydrolyzed to obtain 2, 4,6‑Trinitro‑1,3,5‑triaminobenzene. Since the raw material used in the preparation method is cheap 2,4,6-trinitrotoluene, and the reactants or catalysts used are common products in the chemical industry, the preparation method has the advantages of low cost and simple raw materials. Easy to get features. In addition, the preparation method also has the characteristics of short synthesis steps, simple operation of each step, high yield, fast reaction rate, and easy separation and collection of intermediate and final products, which is conducive to the realization of mass production of TATB.

The invention relates to a method for synthesizing an arylseleno-heterocyclic compound. The method comprises the following step: in an organic solvent, under an oxygen condition, by taking heterocyclic aromatic carboxylic acid and diaryl diselenide ether as reaction raw materials, and under the cooperative promotion action of a copper catalyst, a ligand and alkali, performing oxidative decarboxylation coupling reaction, thereby obtaining the arylseleno-heterocyclic compound. By adopting the method, the substrate, namely the heterocyclic aromatic carboxylic acid, and the copper catalyst are cheap and easy to obtain, the substrate range is wide, reaction conditions are simple, the yield and the purity of the product are high, novel synthesis routes and methods are developed for arylseleno-heterocyclic compounds, and the method has good application potentials and study values.

The invention provides a preparation method of glyphosate polymer, in particular to a N-(Phosphonomethyl)iminodiaceticacid catalytic polycondensation method. The preparation method comprises the following steps of: mixing and conditioning proguanil hydrochloride, sulfuric acid and a catalyst into slurry, wherein the catalyst is a compound selected from sodium bisulfate, potassium bisulfate, ammonium hydrogen sulfate and tripolyphosphate; heating the slurry for carrying out an oxidative decarboxylation reaction until no bubble is generated; and adding one of catalysts and uniformly mix with the slurry after the oxidative decarboxylation reaction and heating the uniformly mixed slurry for carrying out a polycondensation reaction until the reaction is finished. The glyphosate polymer of the invention is used for weeding and has the advantages of high efficiency, durability and slow release effect.

The invention relates to a synthetic method of an aryl methyl selenide compound. In an organic solvent, under the oxygen condition, aryl carboxylic acid and dimethyldiselenide are used as reaction raw materials to obtain the aryl methyl selenide compound through oxidative decarboxylation coupling reaction under the joint promoting effect of a copper catalyst, a ligand and alkaline. The aryl carboxylic acid and the copper catalyst adopted in the method are cheap and easy to obtain, a substance range is wide, the reaction condition is simple, the product yield and purity are high, a new synthetic route and method is developed for the aryl methyl selenide compound, and the aryl methyl selenide compound has good utilization potential and a research value.

The invention discloses a high-efficiency Δ 9,11 A preparation method of canrenone belongs to the technical field of preparation of intermediates of medicines. The method is based on 9α-hydroxy-4-androstenedione as a raw material, and the 9-position hydroxyl group is first eliminated by dehydration reaction to generate Δ 9,11 Double bond, then protect the 3-position carbonyl group, then epoxidize the 17-position carbonyl group, and condense with malonic acid diester to form a lactone ring, and obtain Δ after oxidative decarboxylation or decarboxylation oxidation reaction 9,11 ‑Canrenone, the raw materials of the method of the present invention are cheap and easy to obtain, the cost is low, the reaction products involved in each step are easy to purify, and the total mass yield of the final product is higher than 80%. The method of the present invention has strong operability and extremely high commercial Competitive, suitable for industrialized large-scale production, and has good economic benefits.

The invention discloses a method for preparing atovaquone, which comprises the following steps: taking 4-(4-chlorophenyl)-cyclohexyl-1-methanoic acid and 2-chlorine-1, 4-naphthoquinone as raw materials, generating (3S)-2-chlorine-3-(4-(4-chlorophenyl) cyclohexyl)-1, 4-naphthalenedione by oxidative decarboxylation through a peroxide in the action of a catalyst of silver nitrate, and then obtaining the atovaquone through hydrolysis with alkaline. The method is characterized in that the mixed solvent of acetonitrile and choromethane is used as the solvent for the oxidative decarboxylation and the peroxide is one of the four substances, i.e., sodium persulfate, potassium persulfate, sodium percarbonate and potassium peroxycarbonate. The improved preparation method considerably improves the dissolution of the raw materials in the solvent, raises the rate of conversion, increases the yield, reduces impurities, and significantly enhances the product quality. Therefore, the method is more suitable for industrial production.