36results about How to "The difficulty of the reaction process is low" patented technology

Nitroarylamine compound is prepared with aromatic dinitro compound and through single nitro selecting reduction reaction in organic solvent at normal pressure in the presence of CO and water by using Se as catalyst and alkali as cocatalyst. The said aromatic dinitro compound may have substituent radical in the phenyl radical and the substituent radical may be one or several eletron donating and / or accepting group. The reaction conditions includes the molar ratio between aromatic dinitro compound and water of 1 to 1-1000; molar amount of Se is 0.1-100 % of the aromatic dinitro compound; molar amount of alkali is 0-400 % of the aromatic dinitro compound; the weight ratio between aromatic dinitro compound and solvent of 1 to 2-1000; reaction time of 1-36 hr; and reaction temperature of 20-120 deg.c.

The invention discloses a synthetic method of an ether amine flotation agent. The synthetic method is characterized by comprising the following steps: (1) at ordinary temperature and normal pressure, placing chlorinated alkyl amine hydrochloride and an acid-binding agent in a solvent to sufficiently react and separate out white acicular crystals, adding a drying agent, stirring, filtering and collecting the filtrate; (2) adding a hydride of alkali metals into the filtrate, increasing the temperature till the system is slightly boiled for sufficient reaction; (3) after finish of the reaction, filtering to remove the solvent in the filtrate; (4) adjusting the pH of the filtrate from which the solvent is removed, extracting, separating out an extraction agent layer, and drying to ensure constant weight; (5) adjusting the pH of the dried extraction agent layer, extracting, separating out the water layer, and drying to obtain ether amine hydrochloride; (6) using an inorganic base solution to adjust the pH of ether amine hydrochloride, extracting, separating out an organic layer and removing the solvent in the organic layer to obtain the product. According to the synthetic method, normal-pressure reaction is carried out, the operation is safe, the process is simple and the cost is low.

Arylamine compound is prepared with aromatic nitro compound and through reaction in organic solvent at normal pressure in the presence of CO and water by using Se as catalyst and alkali as cocatalyst. The said aromatic nitro compound may have substituent radical in the phenyl radical and the substituent radical may be one or several electron donating and / or accepting group. The reaction conditions include the molar ratio between aromatic nitro compound and water of 1 to 1-1000; molar amount of Se is 0.1-100% of the aromatic nitro compound; molar amount of alkali is 0-400 % of the aromatic nitro compound; the weight ratio between aromatic nitro compound and solvent of 1 to 2-1000; reaction time of 1-36 hr; and reaction temperature of 20-120 deg.c.

The invention relates to a diselenide compound synthesis method and the adopted technical proposal comprises the following steps: adopting halogenated hydrocarbon and selenium as raw materials and organic base or inorganic base as cocatalyst or no cocatalyst, continuously injecting carbon dioxide gas in organic solvent to react in the present of water under the temperature of 20-100 DEG C at normal pressure for 1-24h, cooling to the room temperature, switching carbon dioxide to air or oxygen to precipitate unreacted selenium, filtrating to collect filtrate, then adding 2-3 times of water, precipitating products and finally obtaining the diselenide compound by filtration. The method invention is normal press reaction with low cost, environmentally friend, low reaction process difficulty, convenient operation and easy following separation of products and catalyst.

The invention discloses a synthesizing method of (S)-N-ethyl-3-[(1-dimethylamino) acetyl]-N-methyl amido phenyl formate, which is characterized by the following: adopting m-hydroxy acetophenone as raw material; synthesizing intermediate 3-(1-(dimethylamino) ethyl) phenol; condensing 3-(1-(dimethylamino) ethyl) phenol and formyl chloride to produce the product with high receiving rate.

The invention provides a process for synthesizing azocompound hydrogenated which comprises, reacting aromatic azocompound in organic solvent under normal pressure at the presence of carbon monoxide and water, using selenium as catalyst, organic bases or inorganic bases as catalyst promoter, synthesizing azocompound hydrogenated in one step, wherein the mol ratio of the aromatic azocompound and water is 1:1-20, the mol amount of selenium is 0.1-8% of the aromatic azocompound, the mol amount of organic base or inorganic base is 0-10% of the aromatic azocompound, the reacting time is 0.5-3 hours, the reaction temperature is 30-100 deg. C.

The invention relates to a method for synthesizing 1-aminoanthraquinone. The technical scheme is as follows: in the presence of carbon monoxide and water, 1-nitroanthraquinone used as a raw material reacts by using selenium as a catalyst and inorganic alkali or organic alkali as a cocatalyst at high temperature under high pressure to synthesize the 1-aminoanthraquinone by one step. The invention is simple and safe to operate, and has the advantages of water-phase reaction, accessible raw material, no pollution, high selectivity and high yield; and after the reaction finishes, the catalyst can be recycled and utilized repeatedly.

The invention relates to a method for synthesizing symmetric urea compounds from nitrocompounds. The technical scheme is as follows: in the presence of carbon monoxide and water, by using nitrocompounds as the raw material, selenium as a catalyst and an organic alkali or inorganic alkali as a cocatalyst (or no cocatalyst is added), reaction is performed under the conditions of atmospheric pressure and no solvent to synthesize the symmetric urea compounds by one step, wherein the mol ratio of water to nitrocompounds is 1:1-1:2.5; the selenium accounts for 0.05-1 mol% of the nitrocompounds; the mol ratio of organic alkali or inorganic alkali to nitrocompounds is 1:10-1:4; the reaction time is 1-8 hours; and the reaction temperature is 35-95 DEG C. The invention is simple and safe to operate, and can synthesize the symmetric urea compounds from the nitrocompounds under the conditions of atmospheric pressure and no solvent by one step, and has the advantages of one-pot reaction, accessible raw material, no pollution, high selectivity and high yield; and after the reaction finishes, the catalyst can be separated and recycled.

The present invention relates to a method used for synthesizing derivatives of 1-alkyl-2-alkoxy-3-indole aldehyde oxime. Indole-one is used as basic material and treated through Vilsmeier-Hacck formylation reaction and alkylation reaction to prepare 1-alkyl-2-chlorine-3-indole aldehyde; under the conditions with potassium hydroxide and fatty alcohol and at the temperature of 50 to 80 DEG C, the reaction is monitored by a thin chromatogram TLC; after the reaction is completed, no treatment is required and hydroxylamine hydrochloride is directly added into the mixture for oximation reaction; the reaction temperature is maintained; the reaction lasts for 1 to 2 hours; the ratio of the 1-alkyl-2-chlorine-3-indole aldehyde, the hydroxylamine hydrochloride, the potassium hydroxide, the fatty alcohol and water is equal to 1mmol to 2mmol to 2mmol to from 5ml to 8 ml to 1ml; finally water is added for sedimentation, and the novel compounds of the category of the 1-alkyl-2-chlorine-3-indole aldehyde can be separated through filtration and chromatography. The method has the advantages of mild reaction conditions, process under atmospheric pressure, simple operation, less investment in the equipment, low production costs, less pollution and high yield.

The present invention relates to a piperazine citrate preparation method, and further provides a piperazine citrate with characteristics of safe quality and good stability. The preparation method comprises that: citric acid and anhydrous piperazine are completely dissolved and filtered, and form a salt in a reaction kettle under an appropriate reaction condition, and cooling crystallization, centrifugation, washing and vacuum drying are performed after the complete reaction to obtain the product. The preparation process has characteristics of simpleness, easy operation, extremely small three-waste generation, high yield, low cost, high product purity, and easy industrial production, wherein the yield is up to more than 90%. In the prior art, the piperazine citrate preparation process comprises adopting citric acid and piperazine hexahydrate as raw materials, adopting water as a solvent, and carrying out dissolving, salt forming, alcohol precipitation, centrifugation and drying, and has disadvantages of complex process, large wastewater generation and low yield. With the present invention, the disadvantages in the prior art are overcome.

The invention relates to a method for synthesizing CLT acid, which has the technical scheme that 2-nitro-4-methyl-5-chlorobenzenesulfonic acid is taken as raw material; under the condition that carbon monoxide and water exist, selenium is taken as catalyst, inorganic base or organic base is taken as catalyst promoter; and reaction is carried out at high temperature and high pressure, so that the CLT acid can be synthesized by a one-step method. The method is simple, convenient and safe, realizes aqueous phase reaction, and is easy in obtaining of raw material, free from pollution, high in selectivity and high in yield; and the catalyst can be recycled after the reaction.

The invention relates to a method for synthetizing mono-thioether compound. The technical scheme adopted by the invention is as follows: in the presence of carbon monoxide and water, disulfide compound and halogenated hydrocarbon compound are used as raw materials, selenium is used as catalyst, organic base or inorganic base is used as cocatalyst or any cocatalyst is not added, the raw materials react in organic solvent at 20-100 DEG C under atmospheric pressure for 1-24 hours, the product is cooled to the room temperature, then carbon monoxide is displaced by air, stirring is performed for 0.2-2 hours, filtration is performed, distilled water and cyclohexane are used to extract the filtrate, and the solvent in the extract liquor is distilled out through reduced pressure distillation to obtain the target product. The method is convenient and safe to operate, adopts one-pot reaction, has common raw materials, no pollution, high selectivity and high yield; and the catalyst can be separated and recycled after the reaction.

The present invention is the synthesis process of hydrogenating aromatic azo compound into hydrogenated azo compounds at normal pressure inside organic solvent in the presence of CO and water as well as Se as catalyst with or without organic or inorganic alkali as co-catalyst. Where, the aromatic azo compound may have substituted radical, and the reaction has molar ratio between aromatic azo compound and water of 1 to 1-20, molar ratio between aromatic azo compound and CO of 1 to 1.1-3, molar amount of Se in 0.1-8 % of aromatic azo compound, reaction time of 0.5-3 hr, and reaction time of 30-100 deg c. The synthesis process is simple and safe, and has easy to obtain material, no pollution, high selectivity, no influence on the sensitive radicals on the aromatic ring, high yield and reusability of the catalyst.

The invention relates to a method for synthesizing 1-aminoanthraquinone. The method includes the following steps that 1-aminoanthraquinone is used as a raw material, in the existence of carbon monoxide and water, sulfur is used as a catalyst, inorganic alkali or organic alkali is used as a promoter, a reaction is carried out under the high-temperature and high-pressure condition, and accordingly the 1-aminoanthraquinone is synthesized at one step. Compared with a selenium-catalyzed reduction method, the sulfur-catalyzed reduction method is lower in cost, higher in productive rate and capable of greatly reducing water consumption.

The synthesis process of benzoyl substituted carbamide compound is the reaction of benzamide and aryl nitro compound in organic solvent inside a sealed high pressure reactor in the presence of CO, Se as catalyst and triethylamine as cocatalyst. Where, the substitutent group of the phenyl group on the aryl nitro compound may be one or several electron donating group and / or electron withdrawing group; the molar ratio between benzamide and aryl nitro compound is 0.1-10; molar amount of Se is 0.1-20% of the minor reactant; molar amount of triethylamine is 10-200% of the minor reactant; the molar ratio between reactant and organic solvent is 0.021-1; the reactio period is 2-20 hr; the reaction temperature is 50-200 deg.C; and the CO pressure is 1-10 MPa gage pressure.