45results about How to "No harsh reaction conditions" patented technology

The invention discloses a preparation method of methyl octabromo-ether and belongs to the technical field of fire retardant methyl octabromo-ether production. The preparation method comprises the following steps: dissolving tetrabromobisphenol A in water, regulating a pH (potential of hydrogen) value with sodium hydroxide, performing heat preservation for the first time, dropwise adding a methallyl chloride organic solution, adding a phase transfer catalyst, after dropwise adding, performing heat preservation for the second time, then cooling to a room temperature, performing lamination, taking an organic layer, dissolving a brominating agent in an organic solvent to form a brominating agent solution, adding the organic layer into a catalyst, dropwise adding the brominating agent solutionfor brominating reaction, performing heat preservation for the third time at 25-55 DEG C, adding a sodium sulfite aqueous solution for reaction, washing with water after the reaction, standing for lamination, taking a lower organic layer, adding into an emolsifier aqueous solution, performing distillation to remove the organic solvent, performing suction filtration to form a material, and drying the material to prepare a product, wherein a mole ratio of the water to tetrabromobisphenol A is (2-8):1; and a range of the pH value is 8-10.

The invention provides a preparation method of an alloy catalyst for degrading formaldehyde. The method comprises the following steps: (1) adding a TiO2 nano material and a cerium compound into water,carrying out impregnation and stirring to disperse cerium onto the TiO2 nano material, carrying out drying, grinding and roasting to obtain a Ce/TiO2 solid material; (2) adding the Ce/TiO2 solid material into water, carrying out stirring until the Ce/TiO2 solid material is completely dispersed, adding a platinum compound, and carrying out impregnation and stirring to disperse platinum onto the Ce/TiO2 solid material; (3) adding an alkali solution as a stabilizer, uniformly carrying out stirring and mixing, then adding a reducing agent, and carrying out a reduction reaction; and (4) separatingthe solid obtained in the step (3), carrying out water washing, alcohol washing, drying and cooling, and then carrying out grinding to obtain the Pt-Ce/TiO2 catalyst. The method is simple and feasible, and no harsh reaction conditions are required. According to the prepared Pt-Ce/TiO2 catalyst, the Pt nano particles are stabilized through the addition of the cerium according to the method, so that the dispersity is improved, the nano particle size is reduced, abundant oxygen vacancies are provided, and formaldehyde can be effectively decomposed.

The invention discloses a synthesizing method of a tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether. The method comprises the following steps: adding tetrabromobisphenol and an alkali into water; stirring until completely dissolving; then carrying out the primary heat preservation; regulating the pH value; adding a dispersing agent; dropwise adding methylallyl chloride and carrying out the secondary heat preservation; after carrying out the primary aftertreatment, obtaining an intermediate product; adding the intermediate product into an organic solvent; stirring until the intermediate product is completely dissolved, and then dropwise adding the bromine; refluxing and carrying out the tertiary heat preservation; and after finishing the tertiary heat preservation, obtaining a product by carrying out the secondary aftertreatment. The method is simple; the adopted solvent can be recycled and reused; the temperature of the bromination reaction is low; the reaction condition is moderate and is easy to control; the energy consumption during the production is low; and the strict reaction conditions are not required by all steps, so that the method is favorable for industrial production. The tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether as the product is high in yield, good in quality, good in heat stability and high in content, thereby lightening the environmental-protection stress. In addition, the tetrabromobisphenol A dual (2,3-dibromo-2-methyl propyl) ether is high in purity, low in impurity content and free of generating 'three wastes' and environmental pollution.

The invention provides a synthesis method of cefepime hydrochloride. The synthesis method comprises the following steps: taking GCLE (7-phenylacetamide-3-chloromethyl-3-cepham-4-carboxylic acid p-methyl-oxybenzyl ester) as a raw material; cutting a 4-site protecting group (p-methoxybenzyl) and enabling the 4-site protecting group to react with N-methylpyrrolidine (NMP); then cutting a 7-site protecting group through an enzyme method to obtain an immediate 7-amino-3-(1-methylpyrrolidine)methyl)-3-cepham-4-carboxylic acid hydrochloride (7-ACP); taking cheap and available methoxyiminoacetic acid mercaptobenzothiazole active ester (AE-active ester) and the 7-ACP to be subjected to 7-site acylation reaction, so as to finally prepare the cefepime hydrochloride. A route provided by the invention can be used for obtaining the high-yield and high-quality cefepime hydrochloride without a delta2 isomer. The synthesis method provided by the invention has the advantages of simple process, no harsh reaction conditions and the like and is very suitable for industrial production.

The invention relates to a method for preparing an anti-tumor medicine imatinib, which comprises the following steps of: performing amidation-condensation two-step 'one pot' reaction on 4-methyl-3-bromaniline (V), 4-(chloromethyl) benzoyl chloride (IV) and N-methyl piperazine to directly obtain a key intermediate N-(4-methyl-3-bromophenyl)-4-(4-methyl piperazin-1-methyl)-benzamide (III); and performing nucleophilic substitution on the N-(4-methyl-3-bromophenyl)-4-(4-methyl piperazin-1-methyl)-benzamide (III) and 4-(3-Pyridinyl)-2-aminopyrimidine (II) to obtain the imatinib (I). The method hasthe advantages that: the process is reasonably designed, expensive reagents are not used, the reaction yield is high, raw materials are low in cost, the operation is simple and convenient, rigorous reaction conditions are absent, and the method is suitable for mass production.

The invention discloses a tetrabromo-benzene anhydride diol synthesis method comprising the steps that: tetrabromo-benzene anhydride and diethylene glycol are uniformly stirred; a catalyst is added; under the protection of a protective gas, fist heating is carried out, and a reaction is carried out when a reaction temperature is reached; when the reaction is finished, an organic solvent is added for dissolving the reaction material; the temperature is reduced, and epoxypropane is added; secondary heating is carried out, and a maintained-temperature reaction is carried out; after the reaction, hot filtering is carried out; and distillation is carried out for removing the organic solvent, such that the product is obtained. The solvent adopted in the invention can be recovered by distillation and can be recycled, the process is simple, reaction temperature is low, reaction conditions are mild, the reactions are easy to control, production energy consumption is low, no harsh reaction condition is in the steps, industrial production can be easily carried out, product yield is high, product thermal stability is high, product content is high, product quality is good, no three-waste production is caused, and no environment-pollution problem is caused.

The invention discloses a novel method for synthesizing 6-bromine-3,4-dihydro-1H-[1,8] naphthyridine-2-ketone and relates to the field of chemical synthesis. The method comprises the following steps:by using a four-step synthesis method, performing hydrogen substitution on a benzene ring on 2-amino-3-hydroxymethylpyridine by using bromine so as to generate 2-amino-3-hydroxymethyl-5-bromopyridine;substituting hydroxyl in the 2-amino-3-hydroxymethyl-5-bromopyridine by using chlorine in thionyl chloride so as to generate 2-amino-3-methyl chloride-5-bromopyridine hydrochloride; carrying out an annulation reaction of the 2-amino-3-methyl chloride-5-bromopyridine hydrochloride by using diethyl malonate so as to generate 6-bromine-3-nonanoic acid-ethyl ester-1,2,3,5-tetrahydro-1,8-naphthyridine-2-ketone; finally, under an alkali condition, removing carboxylic acid carbethoxy from the 6-bromine-3-nonanoic acid-ethyl ester-1,2,3,5-tetrahydro-1,8-naphthyridine-2-ketone, thereby obtaining a final product, namely 6-bromine-3,4-dihydro-1H-[1,8] naphthyridine-2-ketone. The method is low in raw material cost, simple in synthesis process, not harsh in reaction condition, safe and convenient to operate, high in final product yield, and applicable to large-scale industrial production.

The invention discloses a Uio-66/polyaromatic amine composite material with a core-shell structure as well as a preparation method and application thereof. The preparation method comprises the following steps: dispersing Uio-66 in an aqueous solution; adding an aromatic amine monomer and a surfactant, and stirring for 0.5-24 h for sufficient contact; dropwise adding a sulfate aqueous solution to initiate a polymerization reaction, and continuously stirring for 3-24 h; performing centrifugal separation, and washing to obtain a Uio-66/polyaromatic amine composite material. The specific surface area of the composite material reaches 319.77m<2>/g, thereby effectively increasing the specific surface area of polyaromatic amine; moreover, the surface of Uio-66 is subjected to amination modification successfully. The method disclosed by the invention can be used for efficiently preparing the Uio-66/polyaromatic amine composite material, and is economical and effective and easy to operate, andthus has a broad application prospect in the technical field of water treatment.