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30 results about "P-tolualdehyde" patented technology

Oxaphosphaphenanthrene fire retardant containing cyclotriphosphazene and cup [4] aromatic ring structures as well as preparation method and application of oxaphosphaphenanthrene fire retardant

The invention provides an oxaphosphaphenanthrene fire retardant containing cyclotriphosphazene and cup [4] aromatic ring structures as well as a preparation method and application of the oxaphosphaphenanthrene fire retardant. The preparation method comprises the steps that hexa-p-hydroxy phenoxy cyclotripolyphosphazene and DOPO react in an organic solvent to obtain an oxaphosphaphenanthrene intermediate I containing a cyclotriphosphazene structure; p-toluenesulfonate ethoxyl p-tolualdehyde and p-tertiary butyl cup [4] aromatic hydrocarbon react under the action of acetonitrile-K2CO3 to obtain an intermediate II; the intermediate I, the intermediate II and hydrazine hydrate react in the organic solvent to obtain the oxaphosphaphenanthrene fire retardant containing the cyclotriphosphazene and cup [4] aromatic ring structures. The oxaphosphaphenanthrene fire retardant containing the cyclotriphosphazene and cup [4] aromatic ring structures is white in appearance, melting point is 212-214 DEG C, thermal stability is good, flame retardant rate is high, and purity is 99.1%; the used raw materials are available, a technology is advanced, and industrial production can be easily realized. The oxaphosphaphenanthrene fire retardant containing the cyclotriphosphazene and cup [4] aromatic ring structures can be taken as a reactive type fire retardant and can also be taken as an additive flame retardant when being used after being grafted to thermosetting resins of epoxy resin, polyurethane and the like, so as to meet the halogen-free fire retardant requirement of engineering plastics, with high heat resistance requirement on fire retardant, such as ABS, nylon and the like.
Owner:湖北君邦新材料科技有限公司

Novel process of 1,4-bis(methoxymethyl)-benzene preparation method

The invention provides a novel process of a 1,4-bis(methoxymethyl)-benzene preparation method. The novel process comprises the following steps of: (1) reaction distillation: heating low-boiling leftovers containing p-xylylene dichloride to reach the temperature above 110 DEG C, pumping into a reaction kettle under vacuum; adding sodium methoxide solution to react and distil at temperature below 80 to 100 DEG C, stopping reaction to obtain a crude product while the content of the p-xylylene dichloride residual in a reactant accounts for 0.05 to 0.5% (GC), and distilling to obtain methanol; (2) salt dissolving: adding water to the crude product to dissolve salt; (3) heating reflux: heating for 3 to 5 hours to reach 95 to 105 DEG C; (4) standing and layering to obtain an oil layer and a water layer; (5) rectifying: performing reduced pressure distillation to the oil layer to obtain finished 1,4-bis(methoxymethyl)-benzene and a byproduct finished p-tolualdehyde. The novel process is simple, convenient and stable in operation process, active substance can be fully utilized and the generation of three wastes (waste gas, waste water, and industrial residue) is reduced in the process of producing the p-xylylene dichloride.
Owner:QIANJIANG XINYIHONG ORGANIC CHEM

Preparation method of 6-methyl-4-bromo-isoquinoline

The present invention relates to a synthesis method of 6-methyl-4-bromo-isoquinoline. The synthesis method comprises the following steps: using amino acetaldehyde dimethyl acetal and p-tolualdehyde asraw materials, and carrying out a reaction for forming 2,2-methyl-N-(4-methoxy phenyl alkenyl)ethylamine; then adding methyl chloroacetate and trimethyl phosphite to obtain 2,2-dimethoxyethyl((dimethoxyphosphoryl)(p-methylphenyl)methyl)ethyl carbamate; further adding titanium tetrachloride for a reaction, after the reaction traced by a TLC method is completed, further adding a 2N sodium hydroxidewater solution for reaction, then adding diatomite, carrying out stirring and suction filtration, carrying out extraction on the water phase and the filter cake with ethyl acetate, carrying out drying and rotary evaporateion, and carrying out column chromatography purification by using a sufficient amount of silica gel columns of 100-200 meshes to obtain 6-methyl isoquinoline; and adding the 6-methyl isoquinoline into carbon tetrachloride, then adding N-bromo-succinimide, carrying out heating and refluxing for 2-5 hours, concentrating the reaction mixture, carrying out column chromatography with silica gel columns of 100-200 meshes, using petroleum ether PE and ethyl acetate EA as eluants, and carrying out recrystallization with excess petroleum ether to obtain the final product 4-bromo-6-methyl-isoquinoline. The method has the advantages of clear steps, less waste, high yield, raw material conservation and easy operation.
Owner:北京六合宁远医药科技股份有限公司

Synthetic method of procarbazine

The invention discloses a synthetic method of procarbazine (Pcb). The synthetic method comprises following steps: p-tolualdehyde is taken as an initial raw material, dibromocyanuric acid and isopropylamine are added, reaction is carried out at room temperature so as to obtain p-methyl benzoyl isopropylamine; p-methyl benzoyl isopropylamine is dissolved in an organic reagent, N-bromo-succinimide and an initiator are added, heating reflux is carried out, after reaction, the solvent is removed, acetonitrile and a hydrolysis promoter are added, heating reflux is carried out so as to obtain p-formyl benzoyl isopropylamine; p-formyl benzoyl isopropylamine and methylhydrazine sulfate are dissolved in an organic reagent, triethylamine is added for reaction, and the solvent is subjected to rotary drying, sodium cyanoborohydride is added, an obtained reaction system is heated to room temperature, reaction is carried out for more than one night so as to obtain Pcb. According to the synthetic method, bromination is carried out firstly, and then hydrolysis is carried out, p-methyl benzoyl isopropylamine is converted into p-formyl benzoyl isopropylamine, using of strong oxidizing agent and strong acid is avoided, the synthetic method is friendly to the environment, the yield is high, and the total yield of the three steps is 52.9%.
Owner:广州药本君安医药科技股份有限公司

Production method of p-tolualdehyde

The invention relates to a production method of p-tolualdehyde. The method comprises the steps of: pumping a p-xylylene dichloride low-boiling-point compound containing p-methylbenzylidene into a rectifying tower, collecting a p-methylbenzylidene finished product and p-xylylene dichloride finished product fractions; putting the p-methylbenzylidene finished product into an acidolysis reaction kettle, and adding a catalyst and water at the same time; at the end of acidolysis, conveying the lower layer acid water to an acid water storage tank, and pumping an upper layer oil phase into an alkaline hydrolysis kettle; putting Na2CO3 into the alkaline hydrolysis kettle to carry out alkaline hydrolysis reaction, and then pumping the upper layer oil phase into a coarse distillation tower; conducting coarse distillation: subjecting the upper layer oil phase to pressure reduced distillation; performing rectification: putting the collected overhead distillate into the rectifying tower to perform pressure reduced rectification, and collecting 90-115DEG C/30mmHg fractions, thus obtaining a p-tolualdehyde finished product with purity of 99%. The production method of p-tolualdehyde provided by the invention can fully recycle p-methylbenzylidene, realizes zero discharge of process wastewater, has high yield, and can lower the production cost.
Owner:QIANJIANG XINYIHONG ORGANIC CHEM

Production method of p-tolualdehyde

The invention relates to a production method of p-tolualdehyde. The production method comprises the following steps: sucking p-methylbenzylidene-containing p-xylylene dichloride into a rectifying tower under a low boiling condition, and collecting a p-methylbenzylidene finished product and a p-xylylene dichloride finished product fraction; feeding the p-methylbenzylidene finished product into an acidolysis reaction kettle, and adding a catalyst and water at the same time; after acidolysis is completed, conveying acid water on the lower layer into an acid water storage tank, and sucking an oil phase on the upper layer into an alkaline hydrolysis kettle; feeding Na2CO3 into the alkaline hydrolysis kettle, and sucking an oil phase on the upper layer into a crude distillation tower after alkaline hydrolysis reaction is completed; performing coarse distillation: performing decompression distillation on the oil phase on the upper layer; performing rectification: feeding collected fractions at the top of the tower into the rectifying tower for decompression rectification, and collecting a fraction at the temperature of 100 to 110 DEG C per 30 mmHg to obtain a p-tolualdehyde finished product with the purity of 99 percent. According to the production method of the p-tolualdehyde, the p-methylbenzylidene can be fully recycled, and zero discharge of process wastewater can be realized; the yield is high; the production cost can be reduced.
Owner:枣阳市众成化工有限公司
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