34results about How to "Reasonable synthetic route" patented technology

The invention discloses cigarette aroma enhancement humectant 1-L-leucine-1-deoxidation-D-fructose. The structural formula of the cigarette aroma enhancement humectant 1-L-leucine-1-deoxidation-D-fructose is as follows. The invention further discloses a preparation method of the compound. D-mannose is taken as a raw material, and the cigarette aroma enhancement humectant 1-L-leucine-1-deoxidation-D-fructose is successfully synthesized through simple reaction processing. Physical humectant performance tests and inherent sensory quality evaluations show that the humectant has a good physical humectant effect on cigarettes, and can reduce irritation and blended gases of the cigarettes and improve the smoke mellow sense and comfort of the cigarettes.

The invention relates to degradable aqueous polyurethane dispersion and a preparation method thereof. The dispersion comprises the following components in part by weight: 10 to 30 parts of polyol, 15 to 25 parts of diisocyanate, 3 to 8 parts of hydrophilic chain-extender, 1 to 3 parts of collagen, 3 to 5 parts of neutralizer, 45 to 55 parts of acetone, and 140 to 180 parts of deionized water. Themethod comprises the following steps: dehydrating the polyol under reduced pressure; adding the diisocyanate, the hydrophilic chain-extender, the collagen and the acetone into the polyol; reacting the mixture until the isocyano amount reaches a theoretical value; adding the neutralizer and the deionized water into the solution after the solution is cooled; and distilling the product to obtain thedegradable aqueous polyurethane dispersion. Compared with the prior art, the degradable aqueous polyurethane dispersion has the advantages of reasonable synthesis route, simple operation, high product stability, high water resistance, good degradability and sanitary performance, and can be used for package paint of foods, medicaments, cigarettes and other products.

The invention relates to a bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof. The bridged cyclopentadienyl rings of the bis-silicon-bridged dinuclear metallocene compound contain different substituents. Dimethyldichlorosilane reacts with cyclopentadienyl sodium, so that light yellow solution is obtained; the light yellow solution reacts with n-butyl lithium, and dimethyldichlorosilane is then added for reaction, so that bis-silicon-bridged dicyclopentadiene is obtained; the bis-silicon-bridged dicyclopentadiene reacts with n-butyl lithium, halogenide is then added for reaction, n-butyl lithium is then added for reaction, and finally, another halogenide is added for reaction, so that ligand L is obtained; and cyclopentadienyl titanium trichloride or cyclopentadienyl zirconium trichloride or substituetd cyclopentadienyl titanium trichloride or substituetd cyclopentadienyl zirconium trichloride is added in the ligand L, so that the compound is obtained. The synthesis route is reasonable, the yield is high, separation and purification are easy, the amount of needed cocatalysts is less when the compound is used for catalyzing the copolymerization of ethylene, such as ethylene/hexene-1, ethylene/octene-1 and ethylene/decylene, and long-chain Alpha-alkene, the catalytic activity is high, the insertion rate of the long-chain Alpha-alkene is high, and molecular weight distribution is wide.

The invention discloses a novel tobacco humectant 3-O-hydroxyethyl-D-glucose. The structural formula is represented in the invention. The invention also discloses a preparation method of the novel tobacco humectant 3-O-hydroxyethyl-D-glucose. The novel tobacco humectant 3-O-hydroxyethyl-D-glucose is synthesized by taking D-glucose as a raw material, and introducing isopropylidene for protection and deprotection of the hydroxy of D-glucose. It is shown by physical humidity retention test and inner sensory quality evaluation that the humectant possesses excellent physical humidity retention performance on tobaccos, and is capable of reducing tobacco irritation and impure flavor, and increasing mellow flavor and comfortableness of the smoke of tobaccos.

The invention provides a preparation method for (2R,3S)-1-chlorine-3-tert-butoxycarbonylamino-4-phenyl-2-butanol. The preparation method comprises the steps that L-phenylalanine is taken as raw materials, protected by adopting benzyl, esterified and then catalyzed through NMM to generate a mixed anhydride compound, the mixed anhydride compound reacts with diazomethane to generate diazoketone, a reduction reaction and palladium carbon reduction are performed, and finally the intermediate (2R,3S)-1-chlorine-3-tert-butoxycarbonylamino-4-phenyl-2-butanol is obtained. According to the preparation method, the low-cost benzyl is adopted to protect amidogen, the synthetic route is reasonable, the operation technology is simple, safe and high in yield, industrialization can be well achieved, and the production efficiency is improved.

The invention relates to a preparation method of aripiprazole photodegradation impurities, and belongs to the technical field of drug synthesis. According to the preparation method, 2,3-dichlorobenzenamine is taken as a raw material, a compound II is obtained via reaction of 2,3-dichlorobenzenamine with a compound V, and a target product compound I is obtained via reaction of the compound II with a compound III; wherein A in the compound V is used for representing Cl, Br, COOH, CHO, or COCl, A' is used for representing NH2 or NO2, and n is used for representing 1 or 2. The synthesis route of the preparation method is reasonable; the raw materials are easily available; operation is convenient and simple; yield of the target product is high; and purity is high.

The invention discloses a method for preparing Anilofos by recycled ammonium thiophosphate salt from phosphorus-containing wastewater, the method comprises the following operation steps: (1) after themalathion synthesis reaction is finished, quantitative pure water is added into malathion process oil, ammonia water is slowly dripped, and the mixture is left standing for layering to obtain methylsulfide ammonium salt solution; (2) adding p-chloronitrobenzene, acetone, catalyst and solvent methanol into a high-pressure reaction kettle in sequence, and introducing hydrogen to enable the internal pressure to reach 0.20-0.35 MPa; and (3) N-isopropyl p-chloroaniline and chloroacetyl chloride are reacted to generate an intermediate N-isopropyl-N-chloroacetyl p-chloroaniline, and finally N-isopropyl-N-chloroacetyl p-chloroaniline is subjected to solid reaction with methyl sulfide ammonium salt to finally prepare the Anilofos. The method for preparing the Anilofos by the recycled ammonium thiophosphate salt from the phosphorus-containing wastewater is simple to operate, and is green and environment-friendly, and the prepared intermediate of the ammonium thiophosphate salt can be completely used for synthesizing the Anilofos without affecting the quality of the final product.

The invention discloses a method for synthesizing a pyrazole compound based on WK (Willgerodt-Kindler) reaction and VHA (Vilsmeier-Haack-Arnold) reaction. The method comprises the steps that an acyl compound is taken as a raw material to synthesize a carboxylic compound through the WK reaction; a VHA reagent is prepared; the carboxylic compound is added into the VHA reagent to synthesize an oniumsalt condensing agent; the onium salt condensing agent is hydrolyzed to obtain an aldehyde compound; the aldehyde compound is reacted with hydrazine hydrate to obtain the pyrazole compound. The methodhas the advantages that the synthetic route is reasonable, the method is stable and reliable, the synthetic efficiency is high, and the carboxylic compound, the onium salt condensing agent, the aldehyde compound and the pyrazole compound can be obtained simultaneously; the method has wide application prospect and huge commercial value, enriches the variety of inorganic and organic compounds as well as the synthetic method in the inorganic and organic field.

The invention relates to a tedizolid impurity and a preparing method thereof, and belongs to the technical field of drug synthesis. The tedizolid impurity exists in the following tedizolid steps, and please see the steps in the specification, wherein X is fluorine, chlorine, bromine, iodine, tosylate or methanesulfonate, and R is organic boronic acid organic borate ester; and please see the structural formula of the impurity in the specification. The tedizolid impurity is of great significance in deep surveying of the tedizolid. The invention further provides a preparing method which is simple in process.

The invention relates to a preparation method of an HIF-2 alpha inhibitor PT2385. The method comprises the following steps of: performing Friedel-Crafts reaction on p-difluorobenzene serving as a raw material and 3-chloropropionyl chloride to generate an intermediate II, performing substitution reaction on the intermediate II and sodium methyl mercaptide to generate an intermediate III, performing oxidation, reduction and two-step substitution reaction to obtain an intermediate VII, performing oxidation reaction on the intermediate to obtain an intermediate VIII, and reacting the intermediate VIII with n-butylamine to obtain a compound IX, carrying out fluorination reaction and hydrolysis to obtain an intermediate X, and finally carrying out asymmetric reduction reaction to obtain a final product PT2385. Compared with the existing synthesis method, the process route provided by the invention has the obvious advantages that the raw materials are cheap and easy to obtain, the operation is simple and convenient, the number of reaction steps is small, the total yield is up to 47.6%, multi-step high-temperature reaction is avoided, and industrial production is easy.

The invention discloses a preparation method and bioactivity of an amino acid ester compound containing a 4-piperidyl-6-methylpyrimidine heterocyclic ring, which is used for preventing and controllingcucumber mosaic virus, and relates to a compound shown as a general formula (I) and a preparation method thereof. The invention provides the amino acid ester compound containing the 4-piperidyl-6-methylpyrimidine heterocyclic ring, which is synthesized by taking 2-amino-4-piperidyl-6-methylpyrimidine, substituted aldehyde and malonate as raw materials and p-xylene as a solvent through a microwaveone-pot method. The compound I2 provided by the invention has a relatively good inhibition effect on the cucumber mosaic virus and tobacco ralstonia solanacearum. The formula I is shown in the description.

The invention discloses a method of synthesizing an onium salt type condensation agent on the basis on the basis of a Willgerodt-Kindler reaction and a Vilsmeier-Haack-Arnold reaction. The method includes the steps of synthesizing a carboxylic acid compound through the Willgerodt-Kindler reaction with an acyl compound as a raw material; preparing a Vilsmeier-Haack-Arnold reagent; adding the carboxylic acid compound to the Vilsmeier-Haack-Arnold reagent to synthesize the onium salt type condensation agent. The method has reasonable synthesis route and stable and reliable process, is high in synthesis efficiency, can be used for producing the carboxylic acid compound and the onium salt type condensation agent at the same time, has great application prospect and huge commercial value and enriches types of inorganic and organic compounds and synthesis methods in inorganic and organic fields.

The invention discloses a synthesis method of 4-fluoro-5-isopropyl-2-methoxyphenylboronic acid. The method includes: starting from m-fluoroanisole, carrying out reaction with iodine to conduct iodination, then performing catalytic coupling with isopropylboronic acid, finally conducting selective deprotonation/boronation under a large steric hindrance alkali condition, and performing hydrolysis to obtain a product. The method has the advantages of reasonable route design, simple operation and high selectivity, and is suitable for industrial amplification.