40results about How to "The synthesis process is reasonable" patented technology

The invention discloses an aromatic diamine type cyano group-containing benzoxazine resin and its preparation method. The benzoxazine resin belongs to the aromatic diamine type, its monomer main chain contains benzene rings and ether bonds, and the ends of the main chain contain cyano groups. A cured monomer has high heat resistance, high rate of combustion carbon residue, and certain toughness, thus being suitable for manufacturing high temperature resistant and flame retarding materials. The preparation method of the aromatic diamine type cyano group-containing benzoxazine resin takes an aromatic diamino compound, cyano group-containing monohydric phenol and formaldehyde as reaction raw materials to synthesize a benzoxazine monomer, which is then subjected to curing and crosslinking so as to obtain the benzoxazine resin. The monomer of the resin has reasonable synthesis process, high purity, high yield and low cost. And the monomer for synthesizing the aromatic diamine type cyano group-containing benzoxazine resin has a structural formula as the following.

The invention provides a method for preparing weedicide diuron. The method is characterized in that aromatic compound solvents are added in a reaction kettle, cooling and phosgene introduction are carried out, less dimethylformamide is added, 3, 4-dichloro phenylamine solution is dripped, and cocatalyst triethylene-diamine is added after the dripping completion; the temperature is raised to 80 to 100 DEG C, and the stirring is carried out under the heat insulation condition; solution consisting of 3, 4-dichloro phenyl isocyanate and the aromatic compound solvents is obtained through the reaction; and partial solvents are removed through evaporation, then, 40-percent dimethylamine is dripped, and dinitramine is prepared. Because the catalyst dimethylformamide and the cocatalyst triethylene-diamine are used in the reaction in the method provided by the invention, so the total yield of the synthesized dinitramine is higher than 91 percent, and the purity of the dinitramine raw medicine is higher than 99 percent. The synthesis process provided by the invention is more reasonable, the cost is low, the quality is high, a better environment-friendly effect is realized, the safety is higher, the international standard is reached, and the method is more suitable for industrialized production.

The invention provides total-biology-base benzoxazine resin and a preparation method thereof. A monomer of the resin is prepared by reacting dehydroabietylamine as a rosin derivative, biological phenol and paraformaldehyde at the temperature of 85 DEG C with a solution method for 20 hours. The preparation method comprises the following steps: cooling reactants to room temperature, washing with a sodium bicarbonate solution, washing with deionized water, and crystallizing with ethanol to obtain a purified monomer; performing ring-opening crosslinking on the monomer in a heating state or in thepresence of an added catalyst to generate the total-biology-base benzoxazine resin. The total-biology-base benzoxazine resin has the advantages of reasonable synthesis process, no need of inertial gasprotection, high product purity and environmental friendliness; compared with other biology-base benzoxazine and a part of petroleum-base benzoxazine, the obtained novel total-biology-base benzoxazine resin has great competitiveness on the aspects of ring-opening temperature and thermal stability, and shows high corrosion resistance.

The invention discloses a method for preparing diflubenzuron serving as a pesticide. The method is characterized by comprising the following steps of: adding an aromatic compound solvent into a reaction kettle, cooling, introducing phosgene, adding an appropriate amount of dimethyl methanamide, dripping a p-chloroaniline solution and adding triethylene diamine serving as a catalyst promoter; raising the temperature, preserving heat and stirring; reacting to obtain a solution containing rubigan isocyanate and the aromatic compound solvent; and adding 2,6-difluorobenzamide after adding the aromatic compound solvent into another reaction kettle, raising temperature and dripping a p-chloroaniline isocyanate solution to obtain the diflubenzuron. In the method, dimethyl methanamide serving as acatalyst and triethylene diamine serving as the catalyst promoter are used in a reaction, so that the total yield of synthesized diflubenzuron is over 91 percent, and the purity of a diflubenzuron active compound is over 99 percent. The method has the advantages of reasonable synthesis process, low cost, high quality and environmental friendliness, is up to the international standard, and is moresuitable for industrial production.

The invention relates to a preparation method of 1-isopropyl-3-tertiary butyl thiocarbamide, which is characterized by using chlorobenzene as a solvent in the process of preparing the 1-isopropyl-3-tertiary butyl thiocarbamide. The method comprises the following concrete steps: adding tert-butyl isothiocyanate to the chlorobenzene and stirring; cooling, dropwise adding isopropylamine, and insulating and reacting after dropwise adding the isopropylamine to obtain the solution of the 1-isopropyl-3-tertiary butyl thiocarbamide; and after cooling, centrifuging and drying to obtain the 1-isopropyl-3-tertiary butyl thiocarbamide. The invention has safer and simpler technological operation, no three wastes and high yield, and is more environment-friendly and more suitable for industrial production.

The invention relates to a preparation method of arylamine. The preparation method includes dissolving ferric trichloride-water (1/6) in distilled water, and adding dropwise an aqueous solution of sodium hydroxide or potassium hydroxide so that the pH is within the range of 7 to 8; slowly heating the solution so that the temperature is within the range of 55 DEG C to 65 DEG C, preserving heat, leaching, drying filter cakes, and grinding to obtain iron oxide hydroxide powder serving as a catalyst; and adding an aromatic nitro compound, distilled water and the catalyst into a reactor, heating the reactor to the temperature between 60 DEG C and 100 DEG C, adding hydrazine hydrate to react, allowing the reactor to stand, layering, adding an appropriate amount of water, and washing to obtain the arylamine corresponding to the aromatic nitro compound. The preparation method is safe, simple and convenient to operation, few in the three wastes, environment-friendly, high in yield and applicable to industrial production, and the product quality meets national standard.

The invention discloses a method for preparing 2,4-dichloro-5-nitrophenol. The method is as below: first, evenly mixing tris(2,4-dichloro-5-nitrophenyl) phosphate, rare earth trifluoromethyl sulfonate catalyst, a cocatalyst and an alcoholic solvent; then gradually heating to a reflux temperature, reacting for more than 3h; and cooling to room temperature after the reaction, separating the catalyst by filtration, and removing the solvent in a liquid phase by distillation to obtain the 2,4-dichloro-5-nitrophenol. In the presence of the co-catalyst, tris (2,4-dichloro-5-nitrophenyl) phosphate reacts with the alcohol solvent under the catalysis of rare earth trifluoromethyl sulfonate, so as to fundamentally avoid the environmental pollution caused by the large quantities of waste acid in the traditional hydrolysis; the reaction is more thorough; and the method increases the yield of the product 2,4-dichloro-5-nitrophenol from 88% to 98%, increases the purity from 91.5 % to 97.5%, lowers production costs, and plays a positive role for the industrial development of oxadiazon.

The invention relates to a polyester resin impregnating agent which is widely suitable for glass fiber enterprises. The polyester resin impregnating agent is prepared by the following raw materials inparts by weight: 100-200 of dicyclopentanediol, 90-180 of neopentyl glycol, 90-200 of trimethylolpropane, 120-200 of dihydromethyl propionic acid and 70-160 of tetrafluorophthalic anhydride. The invention has high hardness, toughness, tensile strength, bending strength and dissolubility in styrene, trends to refinement in the synthesizing process, improves the feed and temperature control precision and realizes numerical control; the synthesizing process is carried out by from a one-step method to a multistep method so as to enable a molecule chain structure of a polyester film forming agentto be more reasonable and regular, and the molecular weight is as high as more than ten thousand; and the polyester resin impregnating agent is widely applied to the impregnating agent of chopped strand mat, jet, BMC and SMC yarns.

The invention discloses a preparation method for an argatroban intermediate. The preparation method comprises the following steps: subjecting (R)-4-methyldihydrofuran-2(3H)-one to ring opening and then to a reaction with sodium methoxide or potassium methoxide to form R-3-methyl-4-methyl-3-hydroxybutyrate; oxidizing R-3-methyl-4-methyl-3-hydroxybutyrate to form methyl (3R)-3-methyl-4-formylbutyrate; then reacting (3R)-3-methyl-4-formylbutyrate with hydantoin to form (3R)-3-methylene-butyric acid carbomethoxyhydantoin; successively carrying out purification, heating reflux and purification so as to obtain (4S)-4-methyl-2-oxoadipate; reacting (4S)-4-methyl-2-oxoadipate with an amino donor under the action of a catalyst, and carrying out purification so as to obtain (2R,4S)-2-amino-4-methyladipate; reacting (2R,4S)-2-amino-4-methyladipate with methanol, and carrying out purification so as to obtain (2R,4S)-2-amino-6-methoxy-4-methyl-6-oxohexanoic acid; and reacting (2R,4S)-2-amino-6-methoxy-4-methyl-6-oxohexanoic acid with a reducing agent, and carrying out purification so as to obtain the argatroban intermediate. The preparation method of the invention is mild in reaction conditions, low in cost and suitable for industrial production.

In the present invention, TIME group is formed by residue of the following molecular structures, compound II is used to act with developer oxide to release TIME-PUG group when compound is used in developing process, TIME-PUG grou is cracked on TIME-PUG group under certain condition to realease PUG group for improving photographic performance of the film.

The invention provides a benzylthio acetamido acetylpyrazine triazole derivative. A target compound (I) is obtained by condensing a sulfydryl acetamido acetic acid derivative and a benzyl chloride derivative, condensing the condensed derivatives and 2-piperazinone, reacting the obtained condensed product and trimethyloxonium tetrafluoroborate so as to obtain a methoxy imide compound, and carryingout cyclization on the methoxy imide compound and hydrazine, trifluoroaceticanhydride, acetic anhydride, propionic anhydride, trifluoroacetyl chloride, acetyl chloride or acrylyl chloride. The preparation method provided by the invention has the advantages of reasonable design, stable process, easily obtained raw materials for production, no use of high pressure hydrogenation and good production feasibility. By using the benzylthio acetamido acetylpyrazine triazole derivative provided by the invention, dipeptidyl peptidase-IV (DPP-4) can be selectively inhibited; an effect of reducing blood sugar is obtained; and the derivative can be applied to the preparation of drugs for reducing the blood sugar and has the following structural formula (I).