46results about How to "High rate of deuterium" patented technology

The invention belongs to the technical field of deuterium-containing compound synthesis and discloses a synthesis method of an aromatic compound containing a difluorodeuteromethoxy functional group or a difluorodeuterothio functional group. In the presence of an alkali, a difluorocarbene donor, a group shown in the description and heavy water undergo a reaction to produce a deuterated product shown in the description, wherein the difluorocarbene donor is BrCF2PO(OR)2 or (chlorodifluoromethyl)trimethylsilane or (bromodifluoromethyl)trimethylsilane and the alkali is selected from Na, K, Li, Mg, Zn, Al, NaH, KH, LiH, LiAlH4, KOD, NaOD, NaOMe, NaOEt, NaOBu, sodium carbonate, potassium carbonate and cesium carbonate. The method has the advantages of use of cheap and easily available raw materials, simple and mild reaction, high yield, high deuteration rate, and production amplification easiness.

The invention provides a deuterated dimethylhydroxylamine benzoate compound and a preparation method and application thereof. The compound has the following structural formula as shown in the description, wherein R1, R2, R3, R4 and R5 represent hydrogen or , methoxyl or , benzyloxy or, methyl or, phenyl or, fluorine or, chlorine or, bromine or, trifluoromethyl, or oxytrifluoromethyloxy or, nitrylor, cyano or sulfonyl separately and independently; the method comprises the preparation steps that in the presence of inorganic salt, deuterated dimethylamine salt and benzoyl peroxide or a derivative of the benzoyl peroxide are protected from light react in an organic solvent, at 15-35 DEG C without light, reaction is carried out for 15-20 h, and then quenching reaction is carried out; the inorganic salt is alkali metal salt. The compound can be used as a deuterated dimethylamine agent for participating in synthsis of deuterated dimethylamine aryl compounds. A The synthesis strategy has thecharacteristics that the conditions are mild, the yield is high, the reaction rate is high, a the deuterated ratio is high, and the like.

Aiming at the defects and deficiencies in the prior art, the purpose of the present invention is to provide a simple method for the production and preparation of deuterated alcohols or deuterated amines. In the method, heavy water is used as a deuterium source, ketone or imine is used as a reaction raw material, visible light or sunlight is used as an energy source, and the reaction can be efficiently carried out at normal temperature and pressure. Through the selection of deuterium sources, catalysts, electron donors, research on reaction conditions and improvement of reagents used in the reaction, defects such as expensive deuterium sources, dangerous reaction process, harsh reaction conditions, low deuterium substitution rate and poor selectivity in the prior art can be improved. .

The invention provides a method for catalytic conversion of a cyano group into deuterated methyl, a prepared aromatic deuterated methyl compound and an application of the compound. The method comprises the steps as follows: an aromatic cyano compound reacts to produce the aromatic deuterated methyl compound under the action of a metal catalyst with deuterium gas serving as a deuterium source. The cyano group is directly catalyzed into deuterated methyl with the deuterium gas serving as the deuterium source, the operation is simple, the raw material is cheap and easy to obtain, the reaction yield is high, the product deuteration rate is high, and the method can be applied to mass production. The prepared aromatic deuterated methyl compound can be used as a deuterated medicine or can be used for preparation of a deuterated medicine or deuterated medicine composition, and the pharmacokinetics, pharmacodynamics or metabolism toxicity of the medicine can be reduced while the medicine molecular activity is kept unchanged basically.

The invention belongs to the technical field of preparation of deuterated compounds, and particularly relates to a synthesis method of alpha-deuterated carbonyl compounds. Inorganic base barium oxide BaO or barium hydroxide Ba (OH) 2 is used as a catalyst, a deuterium supply reagent is used as a deuterium source, and deuteration of the alpha position of the carbonyl compound is efficiently completed. According to the method disclosed by the invention, the H / D conversion reaction can be carried out at the alpha position of carbonyl at high selectivity without influencing other positions, the applicable substrates are wide, and the target product can be obtained at high yield and high deuteration rate in both cyclic ketone and chain ketone reactions. For the reaction of nitrile compounds and sulfoxide compounds, the target product can be obtained with high yield and medium deuteration rate, and the method has the characteristics of simplicity, high efficiency and good regioselectivity.

The invention provides a method for preparing deuterated aldehydes by using halomethyl compounds as raw materials. Described method comprises the steps: in the solvent that pyridine compound exists and D 2 Add halomethyl compounds to O mixed liquid, and react at 0°C~100°C; then add nitrosobenzene compounds to continue the reaction, and finally the reaction liquid is acidified to obtain the target product. The raw materials used in the method of the present invention are all cheap and easy to obtain, no expensive reagents or heavy metal raw materials are required, and the reaction conditions are simple, without harsh conditions such as high temperature, that is, the preparation method of the present invention is low in cost, simple in operation, and high in deuterium substitution rate. Up to 97%, the target product is easy to purify and the yield is high, up to 95%. Moreover, the substrate of the method of the present invention has wide applicability, and various deuterated aldehyde compounds can be prepared.

The invention discloses a method for preparing a nickel-catalyzed α-deuterated chiral sulfonamide compound. Under an inert atmosphere, a chiral complex is used as a catalyst, and a deuterated alcohol is used as a deuterium source and a solvent. Under ℃, N-sulfonyl imine undergoes asymmetric transfer deuteration reaction to obtain α-deuterated chiral sulfonamide compound; the chemical structural formula of N-sulfonyl imine is: α-deuterated chiral sulfonamide compound The chemical structural formula is: where, R 1 , R 2 , R 3 from C 1 -C 6 Alkyl, aryl, substituted aryl, heterocyclic aryl, R 1 and R 2 Different; the chiral complex is generated in situ by divalent nickel and chiral phosphine ligands. The invention can not only overcome the shortcomings of the existing transition metal catalyzed deuteration reaction, but also has the advantages of environmental friendliness, simple operation, high reaction efficiency, wide substrate applicability and the like.

The invention discloses a catalytic production process of deuterated benzene, which comprises the following steps of: mixing benzene and heavy water according to a volume ratio of 1: 2, and adding platinum on activated carbon; and carrying out sealed heating and stirring reaction at 100-130 DEG C for 8-15 hours, separating, and distilling to obtain the target product deuterated benzene, wherein the platinum carbon is added at a speed of 15-35% / min based on the total weight. A manual powder valve is specially designed for the test, and the adding speed of platinum on activated carbon is controlled through the manual powder valve, so that the influence of the adding speed of platinum on activated carbon into the mixed solution of benzene and heavy water on the deuteration rate of the final target product is researched; and experimental research finds that the deuteration rate of the target product is related to the adding speed of platinum on activated carbon, and when the adding speed of platinum on activated carbon is 15-35% / min, the deuteration rate of the target product is the highest and exceeds 90%.

The invention relates to a method for synthesizing toluene-d8, which belongs to the synthesis technology of deuterated compounds. The pentahalogenated toluene is slowly added to the solvent to obtain a clear solution A; the solution A is transferred to the autoclave, and the deuterated reagent is slowly added to the solution in step 1 under nitrogen protection, and catalyst B is added. A mixed solution C was obtained, filtered and deionized water was added dropwise to obtain a filtrate D; after fractionation, heavy water, catalyst F and zeolite were added, and finally the solution was fractionated, and 110° C. fractions were taken to obtain toluene-d8. In the method, the halo-deuterium exchange reaction on the benzene ring and the hydrogen-deuterium exchange reaction on the methyl group are carried out step by step, which is conducive to the complete deuteration reaction, and the obtained product has a high deuteration rate; the use of the catalyst reduces the consumption of the deuterated reagent, It reduces the production cost and can effectively break the domestic market's dependence on imports.

The invention provides an in-situ synthesized copper nanowire array material and its preparation method and application. The copper oxide nanowire array is placed in a separate two-chamber reaction electrolytic cell, and the copper oxide nanowire array is used as a working electrode in an air atmosphere. Mercury / mercury oxide is the reference electrode, the platinum sheet is the counter electrode, and the electrolytic solution is 0.5M K 2 CO 3 A mixed solution of acetonitrile and deuterated water, wherein the volume of acetonitrile accounts for 30-70% of the total volume of the mixed solution, the volume of deuterated water accounts for 30-70% of the total volume of the mixed solution, and the scanning speed is 8-12mV / s, the scanning voltage is in the range of -0.4--1.4V, and the cyclic voltammetry test is carried out until the reduction peak of copper oxide disappears, that is, the in-situ synthesized copper nanowire array material is obtained. The present invention synthesizes the copper nanowire array (Cu NWAs) material by the method of in-situ transformation, takes the copper nanowire array (Cu NWAs) material as the cathode of the electrochemical reaction, utilizes a kind of simple and convenient electrochemical reduction method to deuterate water The efficient conversion of C-X / C-D is realized for the deuterium source.

The invention provides a deuterated supramolecular polymer, belonging to the technical field of supramolecular polymers. The deuterated supramolecular polymer is a bifunctional monomer with a deuterated polymer as a spacer obtained after ring-opening metathesis polymerization of a deuterated cycloalkene, through quadruple hydrogen bonds or metal coordination bonds. Quadruple hydrogen bonded deuterated supramolecular polymers or metal coordination deuterated supramolecular polymers formed by non-covalent interactions. The invention also provides a preparation method of the deuterated supramolecular polymer. The main chain of the deuterated supramolecular polymer of the present invention is connected to each other through non-covalent interaction, and has the advantages of self-repair and good processing performance. The preparation source of the deuterated supramolecular polymer of the present invention is simple, the process flow is simple, and the preparation of the deuterated supramolecular polymer with a controllable ratio of unsaturated carbon to saturated carbon can be realized by adjusting the type and molar ratio of deuterated cycloalkene , combined with hydrogen isotope addition reactions can adjust the ratio of hydrogen isotopes in the saturated product.

The invention discloses a method for synthesizing chiral amine. According to the method, a catalytic amount of ketone is used as a self-catalyst, alkali which is cheap and easy to get is used as a synergistic catalyst, a 1-aryl-alcoho compound is used as a substrate, chiral methylpropane-2-sulfinamide is used as an amine source, in an inert gas atmosphere, asymmetric amination reaction of alcoholis completed, and through a one-pot method, the chiral amine is obtained. According to the method for synthesizing the chiral amine, a reaction system is simple, operation is simple and convenient, economic benefits are high, transition metal catalysts or other auxiliary additives are not needed, a chiral product does not contain transition metal residues, and the method for synthesizing the chiral amine is clean, safe and efficient; moreover, the target product yield (41%-82%) is high, the stereoselectivity is good (a dr is 99:1), the defects that traditional raw material agents are expensive, a reaction system is complex, synthesis steps are tedious, a deuterated ratio is low, the stereoselectivity is low, and the like are overcome, and the method for synthesizing the chiral amine has very important application prospects in medicine synthesis especially.