124results about "Preparation by N-O/N-N bonds" patented technology

The instant invention provides for novel catiomc lipids that can be used in combination with other lipid components such as cholesterol and PEG-lipids to form lipid nanoparticles with oligonucleotides. It is an object of the instant invention to provide a cationic lipid scaffold that demonstrates enhanced efficacy along with lower liver toxicity as a result of lower lipid levels in the liver. The present invention employs low molecular weight cationic lipids with one short lipid chain to enhance the efficiency and tolerability of in vivo delivery of siRNA.

The present invention provides novel anthracene derivatives. In particular, the present invention provides light-emitting elements with high luminous efficiency, and light-emitting elements with long lifetime. Further, the present invention provides light-emitting devices and electronic devices having long lifetime by using these light-emitting elements. An anthracene derivative represented by the general formula (1) is provided. In addition, since the anthracene derivative represented by the general formula (1) has high luminous efficiency, a light-emitting element using the anthracene derivative represented by the general formula (1) can also have high luminous efficiency. By using the anthracene derivative represented by the general formula (1), light-emitting elements with long lifetime can be provided.

The invention discloses an improved preparing method of anti-parkinson medicine detonate sand java blue important intermediate 2, 3- di-hydrogen- 1H-indenes-1-amine, which is characterized by the following: reacting 2, 3- di-hydrogen- 1H-indenes-1-ketoximes and alumino-nickel in queous alkali getting the product. This invention also discloses a 'one pot boiling' preparing method of 2, 3- di-hydrogen- 1H-indenes-1-amine with 2, 3- di-hydrogen- 1H-indenes-1- ketone. This invention also discloses a 'two steps one pot boiling' preparing method and 'three steps one pot boiling' preparing method of detonate sand java blue with 2, 3- di-hydrogen- 1H-indenes-1-ketoxime and 2, 3- di-hydrogen- 1H-indenes-1- ketone. This invention possesses simple operation, low cost and high productive efficiency, which is fit for industrial production.

It is an object of the invention to provide a novel fungicide which exhibits a wide controlling spectrum against pathogens of various crops, and solves the toleration problem.

The diamine derivative represented by the formula (1) and a process for preparation of the same, fungicides comprising the same as an active ingredient are disclosed:

[wherein R1 is substituents such as an alkyl group having 1 to 6 carbon atoms and the like, R2 and R5 are each independently substituents such as hydrogen atom, an alkyl group having 1 to 6 carbon atoms and the like, R3 and R4 are each independently substituents such as hydrogen atom, an alkyl group having 1 to 6 carbon atoms and the like, or R3 and R4 may be bonded to each other to form a hydrocarbon ring having 3 to 6 carbon atoms, R6, R7, R8 and R9 are each independently substituents such as hydrogen atom, an alkyl group having 1 to 6 carbon atoms and the like, R10 is a substituent such as hydrogen atom, an alkyl group having 1 to 6 carbon atoms and the like, A is an oxygen atom or a sulfur atom, and Q is an aryl group or a heterocycle].

Compounds of formula (I) are prepared by hydrogenolysis of a compound of formula (II):where R1 is haloalkyl, haloalkoxy or -SF5; W is N or CR3; and R2 and R3 are H or Cl. The compounds of formula (I) can be used as intermediates in the preparation of pesticidally active arylpyrazole compounds.

The invention provides a method for economically synthesizing 2,5-diaminotoluene and sulfate of the 2,5-diaminotoluene. The method comprises that: ortoluidine(OT) is subjected to diazonium-coupled reaction under the action of sodium nitrite in inorganic acid water solution to form 2-amino azotoluol(C.I.11160); the 2-amino azotoluol is subjected to reduction hydrogenolysis reaction in the presence of metal or catalyst(Zn or Ni, Pd/C or Raney-Ni), simultaneously the by product of ortoluidine is distilled out by vapor for cyclical utilization, and the 2-amino azotoluol is filtered to synthesize 2,5-diaminotoluene water solution; furthermore, serial products of 2,5-diaminotoluene sulfate(2,5-TDAS) and free 2,5-diaminotoluene(2,5-TDA) of the 2,5-diaminotoluene sulfate are prepared. Due to the adoption of the one-pot in situ synthetic technique, the method has the characteristics of convenient operation, high yield, general equipment, higher recovery circulation rate, easy disposal of waste water, the reduction of waste water discharge by more than 40 percent, effective execution of clean production, generation of circular economy and the like.

The invention provides a resolving and racemization method for 1-amino-1,2,3,4-tetrahydronaphthalene. The method comprises the following steps of: reducing 3,4-dihydro-1-(2H)-naphthalene ketoxime into DL-1-amino-1,2,3,4-tetrahydronaphthalene; and resolving DL-1-amino-1,2,3,4-tetrahydronaphthalene into optically pure (S)-1-amino-1,2,3,4-tetrahydronaphthalene and (R)-1-amino-1,2,3,4-tetrahydronaphthalene by using an acidic resolving agent, or oxidizing chiral secondary amine into corresponding imine or derivatives thereof, reducing into DL-secondary amine and continuously resolving to obtain a single optical product. The enantiomeric excess (ee) value of the obtained product is more than 99.5 percent; and the yield of one-time resolving exceeds 30 percent, and the total yield of the route reaches 46 to 54 percent. Compared with the methods reported by various documents and patents at present, the method has obvious technological and economical advantages.

The invention relates to a method for preparing alkyl-diamine with 1, 8- terpin. It comprises following steps: preparing sulphuric acid solution with mass concentration being 10- 75% at closed condition, adding NaN3 at 10- 15 Deg. C, stirring thoroughly to disslove it in said sulphuric acid solution, then adding 1, 8- terpin, controlling temperature to be between 15-100 Deg. C, stewing, separating and drying after reaction finished and getting diazanyl. The molar ratio between NaN3 and 1, 8- terpin is (2.0- 3.0): 1, the invention employs 5%Pd-C or Lindlar as catalyst to reduce diazanyl and gets alkyl-diamine mixture, distilling, rectifying and getting final product alkyl-diamine. The invention employs NaN3 as raw material, which reduces raw material toxicity, it employs sulfuric acid solution as reaction medium and catalyst, which can be reused when the concentration is moderated, the cost is saved and pollution to enviroment is decreased.

The invention discloses a method for preparing 3-aminomethyl-3, 5, 5-trimethyl cyclohexylamine (isophorone diamine, IPDA) by 3-cyano-3, 5, 5-trimethyl cyclohexanone (IPN, isophorone nitrile), which comprises the following steps: a) 3-cyano-3, 5, 5-trimethyl cyclohexanone and oxyammonia are arranged in an organic solvent for reaction under a temperature ranging from 40 DEG C to 80 DEG C, and 3-cyano-3, 5, 5-trimethyl cyclohexanone oxime is generated; b) 3-cyano-3, 5, 5-trimethyl cyclohexanone oxime, hydrogen and liquid ammonia are arranged in an organic solvent for reaction under a temperature ranging from 50 DEG C to 120 DEG C, a total pressure ranging from 5 MPa to 15 MPa and the effect of a hydrogenation catalyst, and 3-aminomethyl-3, 5, 5-trimethyl cyclohexylamine is obtained. The method has the advantages that, the production of a by-product 3-aminomethyl-3, 5, 5-trimethyl cyclohexanol (IPAA) which is hard to be separated from IPDA is avoided; simultaneously, the amount of liquid ammonia is largely decreased.

The invention discloses trifluoromethyl-substituted azide, amine and heterocycle compounds and preparing methods thereof. The preparing method of the trifluoromethyl-substituted azide compounds includes following steps of: subjecting a trifluoromethylation agent, azidotrimethylsilane and a carbon-carbon double bond of an olefin to addition in an organic solvent under the existence of a catalyst to obtain a compound in which one carbon in the carbon-carbon double bond of the olefin has trifluoromethyl and the other carbon has an azide group. The preparing methods utilize the trifluoromethylation agent which is mild relatively, directly form a carbon-nitrogen bond and a carbon-carbon bond by double-functionalization of olefins, and efficiently synthesize the trifluoromethyl-substituted azide, amine and heterocycle compounds with high selectivity. The preparing methods are easily available in raw materials, mild in reaction conditions, good in atom economy, high in selectivity, simple in after-treatment, environmental friendly, high in yields and suitable for industrial production.

The invention discloses a method for absorbing nitrogen oxide tail gas and generating by-product p-phenylenediamine by using aniline. The method comprises the following steps of: reacting part aniline with NOx to obtain diazonium salt; reacting the diazonium salt with the non-reacted aniline to obtain 1,3-diphenyltriazene, wherein the reaction products contain less p-nitroaniline and o-nitroaniline; making the 1,3-diphenyltriazene in a rearrangement reactor generate the rearrangement reaction at 30 DEG C-120 DEG C to convert into p-aminoazobenzene, wherein 90% of the 1,3-diphenyltriazene is converted into the p-aminoazobenzene and the remaining 1,3-diphenyltriazene is converted into o-aminoazobenzene and few impurities after the rearrangement reaction; separating the low distillates from the rearranged materials; and carrying out the hydrogenation reaction: using Raney nickel as a catalyst, continuously inputting hydrogen gas and controlling the pressure and the temperature to be 0.2MPa-4MPa and 25 DEG C-150 DEG C respectively to synthesize the p-phenylenediamine. The method provided by the invention reduces the production cost of the p-phenylenediamine and also reduces environmental pollution. A DCS (distributed control system) computer control system is used so that the automation of the whole system is realized and meanwhile the production efficiency is high.

The invention relates to a method for synthesizing organic compounds, and provides a method for preparing o-phenylenediamine and a derivative of o-phenylenediamine, for solving the problems that the process route is complex, a great amount of byproducts can be generated and are hard to purify, the reaction condition is rigorous, the environment pollution is severe and the like in a conventional method for synthesizing o-phenylenediamine derivatives. The method disclosed by the invention comprises the following steps: by taking azobenzene and a derivative of the azobenzene as raw materials, synthesizing the o-nitro azobenzene and the derivative of the o-nitro azobenzene under the coactions of a catalyst, an oxidant and a nitrating agent, and further reducing by using a reducing agent, thereby obtaining the o-phenylenediamine and the derivative of the o-phenylenediamine. The method provided by the invention has the advantages that the raw materials are cheap and easy to obtain, the operation is simple, convenient and safe, the synthesis steps are short, the purification is simple, no great waste acid pollution is caused, and the like.

The invention provides a preparation method of 2-aminoindan. Under the catalytic effect of lewis acid such as lithium chloride, aluminium chloride and magnesium chloride, 2-indene oxime is reduced by using potassium borohydride to prepare 2-aminoindan. The synthesis method disclosed by the invention can be completed in one step and has the advantages of less reaction steps, convenient operation, simple separation and purification method and operation, high yield and low cost; the product has good appearance, good color and luster and high purity (99.5%); in addition, the reducing agent used in the method is low in price and easily available; therefore, the preparation method is suitable for industrial production.

The present invention relates to a polymer supported reagent comprising a novel crosslinked mesoporous polymer, enabling a simple and easy production of an azoxy compound or an azo compound from an aromatic nitro compound, and a method of selectively reducing an aromatic nitro compound by using the same. The polymer supported reagent comprises a certain acrylamide mesoporous crosslinked polymer.

The invention discloses a method for preparing 3,3'-dichlorobenzidine hydrochloride by hydrochloric acid translocation. The method comprises the following steps: catalytically hydrogenating ortho-nitrochlorobenzene by hydrogen in the presence of catalysts, such as organic solvents, rare metal and the like to prepare 2,2'-dichlorohydrazobenzene; performing a translocation and rearrangement reactionin hydrochloric acid to finally prepare the 3,3'-dichlorobenzidine hydrochloride with yield reaching over 90 percent. The method has reasonable process route; and the finished product prepared by adopting the method has higher yield and purity, and has larger industrial prospect.

The invention relates to a preparation method of 5,5-dimethyl-1,3-cyclohexamethylenediamine, which comprises the following steps: 1. preparing 5,5-dimethyl-1,3-cyclohexyldione from 4-methyl-3-pentenyl-2-one and diethyl malonate; 2. adding the 5,5-dimethyl-1,3-cyclohexyldione into a polar organic solvent, carrying out condensation reaction with hydroxylamine hydrochloride under the action of an alkaline reagent to prepare 5,5-dimethyl-1,3-cyclohexyldiketodioxime; and 3. adding a polar organic solvent into the 5,5-dimethyl-1,3-cyclohexyldiketodioxime, and carrying out catalytic hydrogenation reduction reaction under the catalytic action of a metal catalyst to prepare the 5,5-dimethyl-1,3-cyclohexamethylenediamine. The total yield of the method is 50-55%, the gas-phase purity and content can reach 98.0% above, and the method has high safety and is simple to operate and beneficial to industrial production amplification.