13 results about "Elimination reaction" patented technology

The application provides a preparation method of dydrogesterone, which comprises the following steps: performing a selective epoxidation reaction on a compound I in a first solution containing meta-chloroperoxybenzoic acid and hydrogen peroxide to obtain a compound II; the content of the meta-chloroperoxybenzoic acid in the first solution is more than 1 times of the amount of substance of the compound I; performing a reduction reaction on the compound II under the action of hydrogen and a catalyst to obtain a compound III; performing a hydrolysis reaction on the compound III in a dilute acid solution, and then performing a hydroxyl elimination reaction on the compound III in a second solution to obtain the dydrogesterone; the structural formulae of the compound I, the compound II, the compound III and the dydrogesterone are as follows:; and. The preparation method has less by-products and a higher reaction yield.

The invention discloses a pyrazolo [5, 1-a] isoindole derivative as well as a synthesis method and application thereof, and belongs to the technical field of organic chemical synthesis. The invention solves the problems of harsh reaction conditions, limited substrate range and the like of continuous multi-step synthesis of a precursor in the existing pyrazolo [5, 1-a] isoindole compound synthesis process. According to the invention, a polarity reversal strategy is adopted, a cyano group is introduced into 1, 5-enyne to change the electronic characteristics of 1, 5-enyne, diazo, olefin and ethynyl benzene are reacted under mild conditions, two rings and three new chemical bonds are constructed through a series of intermolecular [3 + 2] cycloaddition, intramolecular cycloaddition and elimination reactions, and pyrazolo [5, 5-a]-1, 5-a-phenanthrene is efficiently synthesized. According to the present invention, the 1, 1-a] isoindole derivative has characteristics of good synthesis yield, simple operation of the synthesis method, easily available raw materials, good substrate universality and step economy, and provides the effective strategy for the drug design synthesis.

The application discloses a kind of benzindole fluorescent probe compounds and preparation method and application thereof, belong to fluorescent sensing technical field.The benzindole fluorescent probe compound is (E) -3- (4-boronic acid group benzyl) -2- (4-diethylaminostyryl) -1, 1-dimethyl-1H-benzo [e] indol-3-ium.The benzindole fluorescent probe provided in the application uses phenylboric acid as recognition site, can occur selective self-elimination reaction with peroxynitroso anion, to realize the accurate capture and efficient detection of ONOO ‑ With high specific recognition ability.Dual function of viscosity and ONOO ‑ Detection, can be identified and quantitatively analyzed to viscosity change and ONOO ‑ Concentration by fluorescence spectroscopy.The benzindole fluorescent probe compound provided in the application has simple molecular structure, mature synthesis route and easy to scale preparation.

The application provides an intermediate for synthesizing chlorantraniliprole and cyantraniliprole and a preparation method of the intermediate, and the structural formula of the intermediate is 2-amino-3-methylbenzoic acid. The intermediate is obtained by a -D-A reaction, aromatization and a Hoffmann elimination reaction from a cheap bio-based platform compound 2-methylfuran as a starting material. The whole process does not need a dangerous nitration process and a hydrogenation process, the process has mild reaction conditions, good operability, less wastewater and a high yield of the obtained intermediate, and is very suitable for industrialized preparation of an intermediate required by the high-efficiency insecticides chlorantraniliprole and cyantraniliprole.

This invention discloses a method for synthesizing vinylene carbonate. The method includes: reacting chlorovinyl carbonate with triethylamine in the presence of compounds such as oxanthracene or thioxanthracene to generate a vinylene carbonate reaction solution; and then subjecting the reaction solution to vacuum filtration, distillation, and crystallization to obtain electronically pure vinylene carbonate (purity can reach 99.995% or higher). This method can effectively inhibit the polymerization of vinylene carbonate, avoid the formation of vinylene carbonate polymers, improve the yield of the elimination reaction and the overall heat transfer efficiency of the distillation process, reduce the difficulty of separation and purification, and reduce energy consumption, making it suitable for industrial production.

The application relates to the technical field of pharmaceutical chemistry, and discloses a sulfuryl hydrazone compound, a preparation method thereof and anti-tumor application. The compound is synthesized from isatin derivatives and sulfuryl hydrazine through two-step nucleophilic substitution-elimination reaction, has a chemical structure as shown in formula (I), and is characterized by 1H NMR, 13C NMR and HRMS. The sulfuryl hydrazone compound has significant inhibitory activity on A549 (lung cancer), HepG2 (liver cancer) and Hela (cervical cancer) three human cancer cell strains, the value of some compounds is as low as 0.03 micromole / L, the compound can induce cell apoptosis by mediating ROS generation in tumor cells, inhibiting the NF-kappa B signal pathway and activating Caspase-3 activity, and can effectively inhibit cancer cell migration and colony formation. The compound has a mild synthesis process, simple operation and wide substrate applicability, can be used as a potential anti-tumor active ingredient, can be used for preparing drugs for resisting lung cancer, liver cancer, cervical cancer and other tumors, and can provide new candidate compounds and technical support for cancer treatment.

The present application relates to a kind of biological ortho prodrug, composition and its application, specifically disclose a kind of drug prodrug with substituted acrylamide or substituted vinyl sulfonamide structure, is obtained by the reaction of covalent warhead comprising active drug and N-alkyl hydroxylamine.The drug prodrug can be released by Retro-Cope elimination reaction and Cope elimination reaction with tension alkyne, and the release rate can reach more than 90%, to realize on-demand activation active warhead, effectively solve the off-target problem of covalent inhibitor.In addition, by introducing the drug or fluorophore containing hydroxyl / amine group in the propargyl position of tension alkyne, the intermediate produced after Cope elimination reaction of tension alkyne can further undergo elimination reaction, release the drug or fluorophore containing hydroxyl / amine group, realize combined therapy or real-time monitoring of drug release.The above-mentioned drug prodrug and the composition formed by the combination of tension alkyne have good application prospect in the preparation of drug delivery system or active drug.

This invention belongs to the field of fine chemical engineering and organic synthesis technology, and relates to a method for preparing high-purity 1,1-difluoro-2-iodoethylene. The method includes: firstly, in an aprotic organic solvent, under controlled low-temperature conditions, allowing vinylidene fluoride to undergo an addition reaction with iodine monochloride to obtain the intermediate 1-chloro-1,1-difluoro-2-iodoethane; subsequently, the intermediate undergoes a controlled elimination reaction in an alkaline aqueous solution, and the product is immediately removed by reactive distillation, finally purified by distillation to obtain the target product. This invention effectively controls the thermal effect of the addition reaction by introducing a specific solvent, suppressing side reactions such as iodine radical coupling, and eliminating the need for expensive metal catalysts or phase transfer catalysts. The process is simple and safe to operate, with an intermediate separation yield of over 95%, high overall yield, and high product purity, making it suitable for large-scale industrial production.

This invention provides a method for synthesizing triphenylmethylolmesartan medoxomil, an intermediate of olmesartan medoxomil. The method includes hydrolyzing compound 2 in a toluene / C1-C4 lower alcohol mixed solvent under the action of an alkali to obtain a synthesis solution of an intermediate sodium salt; adding a carbonate and a phase transfer catalyst to the synthesis solution of the intermediate sodium salt to carry out a condensation reaction to obtain triphenylmethylolmesartan medoxomil. This invention effectively controls the content of impurity A in the product by using a toluene / C1-C4 lower alcohol mixed solvent system and inhibiting the high-temperature elimination reaction of hydroxyl groups by a protic alcohol solvent. This invention has a short production cycle, a simple process, and does not require changing or adding new solvents during the process, facilitating solvent recovery and reuse in industrial production and effectively reducing production costs. The synthesis method of triphenylmethylolmesartan medoxomil described in this invention has a high overall yield, high production efficiency, simple product purification, and good quality control.

The application provides a synthesis method of deoxycholic acid (DCA). The method takes phytosterol as a starting material, and synthesizes deoxycholic acid (DCA) through a series of steps such as primary alcohol oxidation reaction, witting reaction, hydrogenation reaction, selective reduction reaction, hydroxyl protection reaction, elimination reaction, allyl oxidation reaction and hydrolysis reaction. The synthesis method has high reaction yield and high product purity, the intermediates in each step are all solid, easy to purify, the post-treatment method is simple, the cost is low, suitable for quality control, convenient for industrialized production, and has a good application prospect. Moreover, the deoxycholic acid (DCA) synthesized by the method also avoids the risk of containing animal pathogens and other harmful factors.

Methods for modifying the surface termination of two-dimensional (2D) transition metal carbides (MXenes) are provided. The methods, which allow for versatile chemical modification of the terminating anions via halide exchange or substitution and elimination reactions in molten inorganic salts, provide a processing approach that is widely applicable to MXenes as a broad class of functional materials.

The application provides an olefin polymerization catalyst and a preparation method thereof. The preparation method comprises the following steps: mixing a terminal silicon ether aliphatic amine and a salicylaldehyde compound to perform a condensation reaction, so as to obtain an organic ligand; mixing the organic ligand and silica gel to perform an elimination reaction, so as to obtain an intermediate product A; mixing the intermediate product A and a tetraamine metal compound to perform a complexation reaction, so as to obtain an intermediate product B; and mixing the intermediate product B, a co-catalyst and phenolic aluminum oxide to perform an activation reaction, so as to obtain the olefin polymerization catalyst. The catalyst obtained by the method has high catalytic activity, high metal loading and low cost.

This invention discloses a method for preparing a perfluoroether rubber crosslinking aid. The invention provides a method for preparing a compound as shown in Formula I, comprising the following steps: in an organic solvent, in the presence of a metal reagent, a compound as shown in Formula II undergoes an addition-elimination reaction with tetrafluoroethylene to generate the compound as shown in Formula I. The preparation method provided by this invention has short synthetic steps, uses inexpensive and readily available reagents, and has a high product yield, showing potential for large-scale engineering preparation.