330 results about "Bromobenzenes" patented technology

The invention discloses a crown ether functionalized covalent organic framework material as well as a preparation method and application thereof, and the method comprises the following steps: adding a covalent organic framework material, 4-bromobenzo-15-crown-5, potassium carbonate and potassium iodide into an acetone solution for reaction, washing the obtained crude product, performing Soxhlet extraction with tetrahydrofuran for a certain time, and drying to obtain the crown ether functionalized covalent organic framework material. The crown ether functionalized covalent organic framework material is obtained. Compared with a synthesis method of crown ether functionalized COFs in the prior art, the method has the advantages that the crown ether (4-bromobenzo-15-crown-5) can be grafted to the COFs in one step, the Na < + > adsorption capacity and the adsorbent recycling performance are greatly improved, the synthesis method is simple, and synthesis of the crown ether functionalized COFs is greener, more convenient and more economical.

The present invention relates to a fluxapyroxad intermediate trifluoronitrobiphenyl synthesis method, and belongs to the technical field of organic synthesis, the method comprises the following steps: Step 1: under nitrogen protection, adding 3, 4, 5-bromotrifluorobenzene, o-nitrophenylboronic acid, a catalyst, a promoter, an alkali and a solvent into a reaction flask, and after addition, carrying out a heat preservation reaction; and Step 2: after the reaction is finished, carrying out phase splitting and organic phase concentration to obtain the 3 ', 4', 5 '-trifluoro-2-nitrobiphenyl. Compared with a traditional synthetic method of the trifluoro-nitrobiphenyl, the synthetic method of the trifluoro-nitrobiphenyl has the advantages that the 3, 4, 5-trifluoro-bromobenzene and the o-nitrophenylboronic acid are directly used as raw materials, the production step of preparing the 3, 4, 5-trifluoro-phenylboronic acid from the 3, 4, 5-trifluoro-bromobenzene through a multi-step reaction is avoided, the yield can be effectively improved, the utilization rate of the raw materials is high, and the method is suitable for industrial production. And the o-nitrophenylboronic acid preparation method is simple, the reaction cost can be effectively reduced, the reaction route is shorter, simpler and more efficient, the reaction conditions are mild, and the method has higher industrial application value.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of metaraminol bitartrate. The preparation method comprises the following steps: reacting benzyloxycarbonyl-L-alanine serving as a raw material with dimethylhydroxylamine hydrochloride, then reacting with 3-benzyloxybromobenzene, then carrying out one-step hydrogenation reaction to obtain m-hydroxylamine, and finally salifying to obtain the metaraminol bitartrate. The method adopts a one-step hydrogenation method to simultaneously realize dual effects of reduction and deprotection, reduces operation steps and material consumption, saves material cost, and reduces generation of reaction wastes; in the preparation process, reaction conditions are mild, safety and reliability are achieved, operation is easy, and the obtained target product is high in yield, good in selectivity and suitable for large-scale production.

The invention discloses a preparation method of alplsutentan and an alplsutentan intermediate, alplsutentan is obtained by taking a compound SM1 as a raw material through a one-step method or a multi-step method, and the multi-step method comprises the following steps: reacting the compound SM1 with a compound SM2 to obtain an intermediate I; reacting the intermediate I with 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to obtain an intermediate II, or reacting the intermediate I with ethylene glycol to obtain an intermediate I-b, and then reacting with 5-bromo-2-chloropyrimidine or 5-fluoro-2-chloropyrimidine to obtain the intermediate II; and finally, removing a protecting group from the intermediate II to obtain alpoxivan. The one-step method comprises the following steps: when X in a compound SM1 is a fluorine atom, the compound SM1 is 5-(4-bromophenyl)-4, 6-difluoropyrimidine, and the compound SM1 reacts with sulfonamide and 2-[(5-bromo-2-pyrimidinyl) oxy] ethanol to directly obtain alpoxivan. The synthesis route is short, and the reaction conditions are mild.

The invention discloses a synthesis process of chiral cyclic ether indole. The synthesis process comprises the following steps: reacting 4-bromobenzaldehyde with malonic acid under the catalysis of piperidine to generate olefin carboxylic acid CHP-1; carrying out condensation reaction to prepare CHP-2; under the catalysis of a copper reagent, carrying out Michael addition reaction to obtain CHP-3; preparing a chiral alcohol intermediate CHP-4 through a reduction reaction; trifluoromethanesulfonic acid is used, and a chiral ether intermediate CHP-5 is prepared through ring closing; reacting with protected hydrazine by using a copper ion catalyst to obtain an intermediate CHP-6; the method comprises the following steps: by taking alcohol as a solvent, adding strong acid, and removing a protecting group of hydrazine to obtain an intermediate CHP-7; and carrying out ring closing by taking lewis acid as a catalyst to obtain an indole product CHP-8. The use of a noble metal catalyst palladium is avoided, and the cost is greatly reduced. The chiral center is directly constructed through a chemical method, and SFC is not needed for resolution, so that the cost is remarkably reduced, and industrial production is successfully realized.

The invention relates to the technical field of chemistry, in particular to a synthesis process of 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride, which comprises the following steps: by taking 4-fluoro-3, 5-dimethylbromobenzene as a raw material and hydrazine hydrate as a hydrazine source, matching with alkali such as potassium hydroxide, sodium hydroxide or potassium phosphate and the like, reacting at the temperature of 60-80 DEG C to obtain the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride. The preparation method comprises the following steps: by taking copper or nickel source catalysts such as cuprous bromide, cuprous iodide, nickel salicylate and the like, N, N-bis (2, 6-dimethylphenyl) oxamide as a ligand, hexadecyl trimethyl ammonium bromide as a stabilizer and a dioxane-water mixed system as a solvent, reacting at 80-110 DEG C under the protection of nitrogen, separating a reaction mixed solution after the reaction is finished, and separating the reaction liquid to obtain the target product. And purifying to obtain a finished product of the 4-fluoro-3, 5-dimethyl phenylhydrazine hydrochloride. Therefore, the problems that the synthesis of the 4-fluoro-3, 5-dimethylphenylhydrazine hydrochloride is poor in safety, low in production efficiency, poor in environmental friendliness, small in substrate application range and the like are solved.

The invention discloses a method for synthesizing a platinum-based nitrogen-doped graphdiyne catalyst based on an atomic layer deposition technology and application of the platinum-based nitrogen-doped graphdiyne catalyst. Firstly, hexabromobenzene and calcium carbide are subjected to vacuum ball milling, calcination and purification to obtain a graphdiyne carrier, then the graphdiyne carrier and melamine are mixed and calcined to achieve nitrogen doping of the carrier, and then loading of platinum nanoparticles is accurately controlled through an atomic layer deposition technology. According to the method, the characteristics of an atomic layer deposition technology are utilized, deposition parameters and the number of cycles are controlled, uniform distribution and size control of Pt nano-particles on porous graphdiyne are achieved, and a nitrogen-doped graphdiyne carrier and the platinum nano-particles have a synergistic effect. The platinum-based nitrogen-doped graphdiyne catalyst prepared by the invention has the specific surface area of 734.8 m < 2 > g < 1 > and the average pore size of 8.68 nm, and shows excellent electrocatalytic activity and dynamic performance in reaction.

The present invention discloses a covalent organic polymer fluorescent probe, and the preparation method is as follows: 2,7-dibromopyrene and 1,2,3,4,5,6-hexa(4-bromophenyl)benzene are added to an organic solvent to dissolve, a Ni(0) catalyst is added, and the reaction is heated overnight. After the reaction is completed, it is cooled to room temperature, an HCl aqueous solution is added, the resulting precipitate is filtered, and washed with an organic solvent to finally obtain the covalent organic polymer fluorescent probe. The fluorescent probe is synthesized by a nickel-catalyzed Yamamoto reaction, has a significant quenching effect on nitro explosives containing OH groups, can be observed with the naked eye to have a significant color change, has high sensitivity, and has a low detection limit; and has no significant response to nitro explosives containing OH groups. Therefore, this fluorescent probe can be used as a specific fluorescent probe for highly selective detection of nitro explosives containing OH groups.

The present invention provides a paroxysmal hemoglobinuria indication drug ipropam key intermediate synthesis method, and relates to the technical field of ipropam, the method comprises: taking p-bromobenzaldehyde as an initial raw material, adopting an S-configuration catalyst to obtain an intermediate 03, carrying out protection group removal on the intermediate 03, carrying out automatic ring closing to obtain an intermediate 04, and carrying out post-treatment to obtain the paroxysmal hemoglobinuria indication drug ipropam key intermediate. Reducing the intermediate 04 with sodium borohydride to obtain a single cis-configuration intermediate 05, then carrying out a chiral flip reaction and hydrolysis to remove p-nitrobenzoic acid, then carrying out an etherification reaction with diethyl sulfate to obtain an intermediate 08, reducing amide of the intermediate 08 with sodium borohydride and boron trifluoride diethyl etherate to obtain an intermediate 09, then carrying out an acetylation reaction to protect amino, and finally carrying out a reaction to obtain the chiral cis-configuration intermediate 03. Cuprous cyanide is subjected to a cyanation reaction and a hydrolytic esterification reaction to obtain the ipropam key intermediate TM. The method is low in raw material price, high in chiral control selectivity, easy in reaction condition control and low in equipment requirement, avoids column chromatography and other operations, and is more suitable for industrial production.

The invention discloses an easily degradable modified agricultural mulching film and a preparation method thereof, and relates to the field of high polymer materials. When the easily degradable modified agricultural mulching film is prepared, oyster shell powder sequentially reacts with 3-bromopropyltrimethoxysilane, 4-methylpyridine, 5-(7-bromobenzo [C] [1, 2, 5] thiadiazole-4-yl) thiophene-2-formaldehyde and 4-(diphenylamine) phenylboronic acid pinacol ester, and functionalized oyster shell powder is prepared; and reacting urea with formaldehyde, reacting with monopotassium phosphate and chitosan, mixing with the functionalized oyster shell powder, performing injection molding, and drying to obtain the easily degradable modified agricultural mulching film. The easily-degradable modified agricultural mulching film prepared by the invention has good mechanical properties and capabilities of resisting bacteria, performing photocatalytic degradation, adjusting the pH value of soil and degrading the soil into fertilizers.

The invention discloses a 1, 3, 5-tri (1 '-methylene-3'-vinyl imidazole) benzene functionalized hydrothermal bamboo charcoal adsorption material and a preparation method and application thereof.The preparation method of the adsorption material comprises the steps that bamboo powder, 1, 3, 5-tri (1 '-methylene-3'-vinyl imidazole bromine) benzene, azodiisobutyronitrile and a solvent are evenly mixed and then subjected to a hydrothermal reaction, and the 1, 3, 5-tri (1 '-methylene-3'-vinyl imidazole bromine) benzene functionalized hydrothermal bamboo charcoal adsorption material is obtained. After the reaction is finished, the 1, 3, 5-tri (1 '-methylene-3'-vinyl imidazole) benzene functionalized hydrothermal bamboo charcoal adsorbent is obtained. The prepared adsorbent can effectively adsorb anion pollutants, the highest adsorption capacity of methyl orange at room temperature can reach 605mg / g, the highest adsorption capacity of 2, 4-D Na can reach 338mg / g, and the adsorbent can be recycled and has a good application prospect.

The invention provides a synthesis method of an OLED polycyclic fused thiophene compound, and relates to the technical field of material synthesis, and the synthesis method comprises the following steps: providing and mixing 2-naphthalene sulfonic acid and dichloromethane, dropwise adding an N-bromosuccinimide solution into the mixture under the protection of inert gas, and reacting to obtain an intermediate A; dissolving the intermediate A, then adding sodium hydroxide, 4-bromophenylboronic acid, water and tetrakis (triphenylphosphine) palladium, and reacting to obtain an intermediate B; dissolving the intermediate B, adding sulfonic acid and phosphorus pentoxide, and reacting to obtain an intermediate C; adding the intermediate C into tetrahydrofuran, dissolving, adding lithium aluminum hydride under inert gas, and reacting to obtain a target compound. According to the method, the chemical reaction efficiency of the intermediate C is high, and the yield and LC purity of a target product are relatively high.

The invention discloses benzo [4, 5] imidazo [2, 1-a] isoquinoline compounds as well as a preparation method and application thereof, and belongs to the technical field of biological medicines. The benzo [4, 5] imidazo [2, 1-a] isoquinoline compound can be used for preparing anti-tumor (human breast cancer) drugs, the structure of the benzo [4, 5] imidazo [2, 1-a] isoquinoline compound is shown in the specification, in the formula, R1 is any one or two of hydrogen, halogen, alkyl, alkoxy, fused ring and aryl; r2 is any one of hydrogen, halogen, alkyl and alkoxy; and R3 is any one or two of hydrogen, halogen, alkyl and alkoxy. The preparation method of the compound comprises the following steps: by taking palladium acetate and norbornene as catalysts, tris (4-chlorphenyl) phosphine and the like as ligands, potassium carbonate and the like as alkali and 1, 4-dioxane as a solvent, carrying out one-pot synthesis on a 1-(2-bromo-1-phenyl vinyl) benzimidazole compound and an iodobenzene compound in an argon atmosphere. Structure of compound: # imgabs0 #

The invention provides ester group functionalized cyclotriveratrum hydrocarbon as well as a preparation method and application thereof, and relates to the technical field of gas chromatographic analys.According to the ester group functionalized cyclotriveratrum hydrocarbon and the preparation method and application thereof, a long alkyl chain and an ester group are introduced to the lower edge of cyclotriveratrum hydrocarbon, so that the property of the cyclotriveratrum hydrocarbon serving as a gas chromatographic stationary phase is improved; by introducing a non-polar alkyl chain and a polar ester group, the melting point of the cyclotriveratrum hydrocarbon can be reduced, the film-forming property and the thermal stability of the cyclotriveratrum hydrocarbon are improved, and the separation performance of the cyclotriveratrum hydrocarbon serving as a stationary phase of a capillary gas chromatographic column on an analyte is improved; the method can effectively separate methyl benzaldehyde isomers, bromobenzaldehyde isomers, nitrobenzaldehyde isomers, diethylbenzene isomers, benzene series, homologues, cis-trans isomers and multi-component complex mixtures.

The invention relates to the technical field of catalytic synthesis, in particular to a chloromethylation catalyst, a preparation method of the chloromethylation catalyst and a method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene through the chloromethylation catalyst, and the chloromethylation catalyst is prepared by loading sulfonic acid compounds and (or) pyridine compounds and (or) copper salt on a molecular sieve. The method can improve the localization selectivity of chloromethylation. The method for preparing high-purity ortho-position, meta-position and para-position chloromethyl styrene comprises the following steps of: reacting beta-bromophenylethane, paraformaldehyde and lewis acid in the presence of the chloromethylation catalyst to generate chloromethyl beta-bromophenylethane, and then performing elimination reaction under an alkaline condition to generate a chloromethyl styrene crude product; the high-purity ortho-position, meta-position and para-position chloromethyl styrene is obtained after the crude product is rectified, the brand-new catalyst is adopted in the method, the reaction selectivity is enhanced, the process is simple, and industrial production is facilitated.

The present invention relates to 7-(4-bromophenyl)-2-oxo-9-(trifluoromethyl)-1,2-dihydro-4- hydroxypyrido[3',2':4,5]thieno[3,2-d]pyrimidin or a pharmaceutically acceptable salt, hydrate or solvate thereof, or a hydrate or solvate of a salt thereof, as well as a pharmaceutical composition comprising the same, for use in treating advanced or metastatic cancer with mutations in homologous recombination genes.

The invention discloses an 8-bromine-5-substituted-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole derivative, and the 8-bromine-5-substituted-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole derivative is 8-bromine-5-(4-chlorophenethyl)-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole and / or 8-bromine-5-phenethyl-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole. The invention further discloses a preparation method of the 8-bromine-5-substituted-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole derivative. The 8-bromo-5-substituted-1, 3, 4, 5-tetrahydrothiapyran [4, 3-b] indole derivative provided by the invention has the effects of inhibiting rhizoctonia solani and promoting seed germination. The compound provided by the invention not only can be used for preventing and treating rice sheath blight disease through spraying treatment, but also can be used for preventing rice seeds from carrying bacteria in a seed soaking manner, so that the rice sheath blight disease is comprehensively prevented and controlled. Besides, rice seeds are soaked in a compound solution, germination of the rice seeds can be promoted, the root length, growth vigor and fresh weight indexes of the seeds are improved, and the compound has good application prospects and value in prevention and treatment of the rice sheath blight disease.

This invention discloses an analytical method for benzothiazole contaminants, comprising the following steps: detection by high performance liquid chromatography (HPLC), with the following chromatographic conditions: a phenylhexyl column as the stationary phase, mobile phase A being water, mobile phase B being acetonitrile, and gradient elution; wherein the benzothiazole contaminants are at least one of 2-aminobenzothiazole, 2-hydroxybenzothiazole, benzothiazole, 2-methylbenzothiazole, 2-mercaptobenzothiazole, 2,5-dimethylbenzothiazole, 2-cyanobenzothiazole, ethyl 2-carboxylate benzothiazole, 2-chlorobenzothiazole, 2-bromobenzothiazole, 2-methylthiobenzothiazole, phenylthiocyanate, N-tert-butyl-2-benzothiazole sulfenamide, 2-(2-hydroxyphenyl)-benzothiazole, N-cyclohexyl-2-benzothiazole sulfinamide, dibenzothiazole disulfide, and N,N-dicyclohexyl-2-benzothiazole sulfonamide.

The invention discloses a method for preparing 3-phenanthrenol. The method comprises coupling a compound 3-tert-butoxyphenylboronic acid and o-bromobenzaldehyde to obtain 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, then reacting 2-(chloromethoxy)-2-methylpropane with magnesium chips in tetrahydrofuran to generate a Grignard reagent, followed by substitution with 3'-tert-butoxy-[1,1'-biphenyl]-2-formaldehyde, and reflux and water separation with p-toluenesulfonic acid to obtain 3'-tert-butoxy-2-(2"-tert-butoxyvinyl)-1,1'-biphenyl, and finally ring closure with methanesulfonic acid and de-tert-butylation to obtain 3-phenanthrenol. The method introduces tert-butyl protection, thereby increasing steric hindrance and reducing isomers during ring closure, and facilitating deprotection conditions. The obtained product can have a purity of more than 99.0% without the need for column chromatography.

The application relates to a metal organic tetrahedral cage compound, a preparation method and application thereof, and belongs to the technical field of fine chemical industry. The metal organic tetrahedral cage compound is obtained by reacting a rare earth metal cerium salt with H4BPDS as a ligand 3+ As a node, H4BPDS is used as a ligand. The metal organic tetrahedral cage compound prepared by the application has low raw material price, high yield, stable chemical properties, and can efficiently catalyze the reaction of aryl iodide and aryl sulfinate to prepare diaryl sulfone derivatives under mild light and warm conditions. For the catalysis of the reactions of 4-bromo-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 4-bromophenyl-4-methylphenyl sulfone, 3-bromo-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 3-bromophenyl-4-methylphenyl sulfone, and 4-bromo-3-fluoro-iodobenzene and 4-methylphenyl sulfinate sodium to prepare 4-bromo-3-fluorophenyl-4-methylphenyl sulfone, the yield can reach 95% at the highest.

The invention relates to a pinoxaden preparation method, which comprises: S1, carrying out a cyclization reaction on hydrazine hydrate and a compound represented by a formula (I) to generate an intermediate 1; s2, reacting the intermediate 1 with a compound as shown in a formula (II) in the presence of alkali to generate an intermediate 2; s3, enabling the intermediate 2 to react with 2, 6-diethyl-4-methyl bromobenzene under the action of a catalyst to generate an intermediate 3; s4, the intermediate 3 and pivaloyl chloride react in the presence of alkali, pinoxaden is obtained, the structural formula of the intermediate 1 shown in the formula (I) is shown in the description, the structural formula of the intermediate 2 shown in the formula (II) is shown in the description, and the structural formula of the intermediate 3 shown in the description is shown in the description.

The invention belongs to the field of medicinal chemistry, and relates to an indole allylamine amide derivative as well as a preparation method and application thereof. Functional activity screening of G protein dependent signaling pathways is carried out on all the synthesized compounds, and it is found that the new derivatives can be used for preparing beta2-adrenergic receptor allosteric antagonism regulator drugs. Trans-indole allylamine is used as a raw material, amide coupling is performed to obtain the novel indole allylamine amide derivative, and R1 is any one of phenyl, m-methylbenzene, m-methoxyphenyl, m-bromophenyl, m-chlorphenyl, m-fluorophenyl, o-methoxyphenyl, p-methoxyphenyl, naphthalene ring, oxazole, cyclohexyl, cyclopentyl, methyl, ethyl and isopropyl. A biological activity test result shows that the indole allylamine amide derivative disclosed by the invention has relatively good antagonistic activity on beta2AR and can be used for carrying out negative allosteric regulation on the functional activity of isoproterenol.

A quinazolinone catalyst with both N-N and C-C axis chirality and its synthesis method and application, its chemical structural formula is shown in Formula 4; Synthesis method: using indole-derived o-aminobenzamide and 1-naphthaldehyde derivative as raw materials, using molecular sieve as dehydrating agent, bromobenzene as reaction solvent, stirring for 4h under the catalysis of chiral phosphoric acid and 10°C, then adding ethyl acetate, 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, stirring for 10h under room temperature, TLC tracking reaction to complete formula 3 compound; using formula 3 compound, phenylsilane, trifluoromethanesulfonic acid as raw materials, adding toluene, stirring reaction under 100°C, TLC tracking reaction to end to obtain formula 4 compound. The catalyst prepared by the present invention can be used as a chiral ligand in transition metal-catalyzed asymmetric allylation reaction, with excellent stereoselectivity control effect; the method has mild reaction conditions, low cost and high enantioselectivity.

The invention discloses a dicarbazole bipyridine compound as well as a preparation method and co-sensitization application thereof, and the specific preparation process comprises the following steps: dissolving a compound as shown in a formula II and 4-pyridylboronic acid in a solvent, adding an alkaline substance and a catalyst, carrying out heating reflux reaction under stirring, and after the reaction is finished, carrying out post-treatment to obtain a compound as shown in a formula DSB-6; the preparation method comprises the following steps: dissolving 4-bromophenylpyridine, bis (pinacolato) diboron, PdCl2 (dppf) and potassium acetate in 1, 4-dioxane, heating and refluxing, then adding a compound as shown in a formula II, an alkaline substance aqueous solution and a catalyst, heating and refluxing to react while stirring, and after the reaction is finished, carrying out post-treatment to obtain a compound as shown in a formula DSB-7, and using the compound as a dye sensitizer to prepare the dye sensitizer. According to the preparation method disclosed by the invention, an alkyl chain is connected with dicarbazole and bipyridine, and benzothiadiazole or phenyl benzothiadiazole is introduced into carbazole, so that the dicarbazole and bipyridine compound is synthesized, and a new applicable substance is added for screening dye sensitizers.

The application discloses a conjugated polymer material capable of realizing neutral state green / black-transparent electrochromic performance and a preparation method and application thereof. The conjugated polymer material (IV) is prepared through copolymerization of a cyclic ether modified p-dibromobenzene ring monomer (I), a thiophene derivative ProDOT monomer (II) and a D-A-D unit ProDOT-BTD-ProDOT coupling monomer (III). The electrochromic polymer thin film processed from the conjugated polymer material has application prospects in the fields of intelligent windows, intelligent glasses, displays, electronic paper and the like. In the material, the cyclic ether modified p-dibromobenzene ring monomer effectively reduces the oxidation potential of the conjugated polymer, improves the electrochromic performance of the black / green-transparent electrochromic thin film, and realizes stable and reversible conversion.

The invention discloses a preparation method of a 3-substituted isocoumarin compound, and belongs to the technical field of coumarin compound synthesizing.The preparation method comprises the steps that a 2-bromophenylboronic acid compound and alkyne serve as reaction substrates, a bidentate nitrogen ligand is added and dissolved in a solvent, under the action of alkali and a copper catalyst, a normal-pressure one-step cyclization reaction is conducted in the CO2 atmosphere, and the 3-substituted isocoumarin compound is obtained. The 3-substituted isocoumarin compound is obtained. According to the method, CO2, alkyne and 2-bromophenylboronic acid are used as reaction raw materials, cheap copper is used as a catalyst, the use amount is small, the 3-substituted isocoumarin is obtained through carbon-carbon coupling-cyclization by a CO2 activation one-step method under normal pressure, the conditions are mild, the cost is low, and the method is environmentally friendly.

The invention discloses a preparation method of a covalent organic framework photocatalyst for photocatalytic reduction of CO2, which comprises the following steps: adding 4, 4 ', 4' '-(1, 3, 5-triazine-2, 4, 6-triyl) triphenylamine and 2, 5-dibromobenzene-1, 2, 4, 5-tetracarboxylic dianhydride into a reaction kettle, then adding 1-hydroxy-3-methylbenzene and isoquinoline, and uniformly mixing; and carrying out microwave heating on the reaction kettle, cooling to room temperature, filtering, collecting precipitate, washing, and then carrying out Soxhlet extraction and vacuum drying to obtain the covalent organic framework photocatalyst. A surface halogen atom modification strategy is designed and used for regulating and controlling electron distribution and light capture capacity of a donor-acceptor (D-A) in TzPm-COF, and results show that the strategy can effectively improve photocatalytic activity and selectivity of reduction of CO2 into CO, and can be applied to preparation of the TzPm-COF catalyst. A reasonable design strategy is provided for developing a functional modified COFs material for efficiently and selectively photocatalytic CO2 reduction.

The invention discloses a preparation process of photoinitiator methyl benzoylformate, which comprises the following steps: carrying out bromination reaction on acetophenone serving as a raw material to obtain 2, 2-dibromo-1-phenylethanone; the method comprises the following steps: carrying out alcoholysis on 2, 2-dibromo-1-phenylethanone in a specific solvent under photocatalysis to obtain high-purity methyl benzoylformate; the preparation process has the advantages of easily available raw materials, mild reaction conditions and simple post-treatment, and is suitable for industrial production.

The invention provides S-fluoroalkyl substituted amino acid, polypeptide and a preparation method of the S-fluoroalkyl substituted amino acid, and belongs to the technical field of fluorinated amino acid. The chemical structural formula of the compound is shown in the specification. Wherein Ar is 4-phenyl phenyl, 4-acetyl phenyl, 4-methoxycarbonyl phenyl, 4-acetoxyphenyl, 4-cyano phenyl, 4-(N, N-dicarboxamide) phenyl, 4-(N, N-dicarboxamide) phenyl, 4-(N, N-dicarboxamide) phenyl, 4-(N, N-dicarboxamide) phenyl, 4-(N, N- Ar'is phenyl, 4-iodophenyl, 4-bromophenyl, 3-methoxycarbonyl phenyl, 2-naphthyl or 3-thienyl, and R1 and R2 are methyl or H. According to the preparation method of the S-fluoroalkyl substituted amino acid and polypeptide, the adopted raw materials are low in cost, simple and easy to obtain, glassware cannot be corroded like other methods, and the tedious and functionalization steps are omitted in the preparation method.

The invention discloses (E)-1, 4-diether olefin and a preparation method thereof, and the (E)-1, 4-diether olefin is obtained by using 1, 3-diene as a raw material and carrying out electrochemical reaction in the presence of an electrolyte and a solvent, wherein the 1, 2, 4-trimethyl-1, 3- The structural formula of the 1, 3-diene is as follows: R1 is phenyl, p-fluorophenyl, p-chlorphenyl, p-bromophenyl, p-methylphenyl, p-methoxyphenyl, p-trifluoromethylphenyl, p-trifluoromethoxyphenyl, p-acetoxyphenyl, p-methyl formate phenyl, p-cyanophenyl, p-pinacol borate phenyl, p-phenylphenyl, o-oxybenzyl phenyl and o-methoxyphenyl; r1 is one of 1, 2-naphthyl; the solvent is a mixed solvent containing methanol. The preparation method of (E)-1, 4-diether olefin has high E-selectivity and 1, 4-selectivity, and an electro-catalysis mode is adopted, so that the use of a stoichiometric toxic, expensive or dangerous oxidant is avoided.