157 results about "Annulation" patented technology

A material for an organic electroluminescence device represented by the following formula (I):

The invention provides a synthetic method of plant growth regulator trinexapac-ethyl intermediate 3-carbethoxy-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate. The synthetic method comprises the following steps: (1) carrying out annulation reaction on 2-acetonyl-1,4-diethyl succinate and organic alkaline at the temperature of 20-120 DEG C for 0.5-5 hours in a non-polarity organic solvent to obtain 3,5-cyclohexanedione-1-ethyl formate; and (2) adding organic amine and cyclopropanecarboxylic acid chloride, and carrying out acylation reaction at the temperature of minus 5-50 DEG C, so as to obtain 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate in the presence of micromolecular alcohol, ether, ketone and nitrile the carbon atoms of which are below C8 and are used as additives. According to the method, special additives are added before acylation so that cyclopropanecarboxylic acid chloride can directly react with intermediate-state 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol sodium salt to obtain the trinexapac-ethyl precursor 3-ethoxycarbonyl-5-oxo-cyclohexane-1-enol cyclopropanecarboxylate, thereby shortening reaction time, simplifying synthesis process and improving yield; and the product is directly rearranged without purification so as to obtain the final product trinexapac-ethyl.

The invention discloses a copolymer containing a zinc-phthalocyanine group on a side chain and a preparation method thereof. The preparation method of the copolymer combines RAFT (reversible addition-fragmentation chain transfer) and a phthalocyanin annulation method for the first time to prepare the copolymer containing a zinc-phthalocyanine group on a side chain, and comprises the following steps of: on the presence of an initiator and a chain transfer agent, performing RAFT polymerization on a monomer methacrylic acid-6-(3,4-dicyanophenoxy)caprolactone to obtain a polymer PMADCE (polymethyl acrylic acid-6-(3,4-dicyanophenoxy)caprolactone) containing a phthalonitrile functional group on a side chain; and using the phthalonitrile functional group on the side chain of the PMADCE as a reaction point to perform phthalocyanin annulation with 4-(octyloxy)phthalonitrile in the presence of a heat-sensitive catalyst and zinc acetate so as to obtain a polymer PMADCE-ZnPc containing the zinc-phthalocyanine group on the side chain. The preparation method is few in step, simple, feasible, convenient in purification process, mild in reaction condition, controllable in process and high in conversion rate; and the PMADCE-ZnPc prepared by the method has good solubility and phthalocyanin functionality, can be used as a photoelectric material, and has good application prospects in solar cells, sensors and information storage.

The present invention discloses the production process of high purity 1, 4-dioxane. Diglycol material is produced into high purity 1, 4-dioxane via dewatering and annulation at 150-200 deg.c in the presence of liquid and solid catalysts; low temperature dewatering via adding azeotrope, and eliminating impurity with added impurity eliminating agent. The present invention has less catalyst consumption, high yield, low cost, and no waste water and waste gas exhausted.

The invention discloses a method for degrading polybrominated diphenyl ether by combining surfactant solubilization and UV technology, which belongs to the technical field of environment-friendly halogenated aryl hydrocarbon organic pollutant treatment. The method adopts the technical proposal that surfactant solubilization of 2,2',4,4',5-pentabromated diphenyl ether is improved in a hydrophobic environment provided by nonionic surfactant micelle (Brij 35 or Brij 38) under the conditions of normal temperature and pressure, water bath and ultrasonic sound; and the 2,2',4,4',5-pentabromated diphenyl ether which is dissolved in a surfactant solution is subjected to UV advanced treatment at normal temperature and pressure and then subjected to stepwise debromination reaction or intermolecular elimination and annulation reaction to generate intermediate products, namely PBDEs from monobromo to tetrabromo and polybrominated dibenzofuran (PBDFs) from monobromo to tetrabromo. The whole technology has short time consumption and high efficiency, and the method can selectively degrade target pollutant without damaging a surfactant, provides convenience for recycling of the surfactant, and has good application prospect in the aspect of remediation of soil polluted by the PBDEs in electronic waste recycling sites.

Benzoxazine resin based carbon aerogel and a preparing method thereof are disclosed. The method includes weighing an amine and paraformaldehyde, adding into a four-neck distillation flask, adding an organic solvent, stirring at room temperature until full dissolution, weighing a phenol monomer, dissolving the monomer into the organic solvent, mixing the obtained solution with the solution mentioned above, stirring, gradually heating to allow the amine, the paraformaldehyde and the phenol monomer to be subjected to an annulation reaction to obtain a benzoxazine solution, heating the benzoxazine solution in an oil bath to cure the benzoxazine solution so as to prepare partially-cured polybenzoxazine wet gel, naturally drying the partially-cured polybenzoxazine wet gel to prepare partially-cured polybenzoxazine aerogel, and subjecting the cured polybenzoxazine aerogel to heat treatment and high-temperature carbonization in an inert atmosphere to prepare polybenzoxazine resin based carbon aerogel. The product has advantages of a short preparation period, a low production cost, low equipment requirements, high safety, and high product purity.

The invention provides an environment-friendly preparation method for a lipid-lowering drug ciprofibrate. The preparation method comprises the following steps of by taking hydroxyphenyl ethene as a raw material, carrying out Bargellini and annulation reaction to prepare the ciprofibrate. Compared with the traditional method, the method has the advantages of less reaction steps, short production cycle and high total yield, is easy to operate, mild and easy-control in conditions, convenient for postprocessing and environment-friendly, and is a brand new method for industrialized synthesis of the ciprofibrate.

A compound represented by the formula (I):

[In the formula, Link represents a saturated or unsaturated straight hydrocarbon chain having 1 to 3 carbon atoms, C² to C⁶ in the aromatic ring (E) independently represent a ring-constituting carbon atom, one of the ring-constituting carbon atoms may be replaced with V, V represents nitrogen atom, or carbon atom substituted with Zx, Zx represents a saturated alkyl group having 1 to 4 carbon atoms and the like, Rs represents -D-Rx etc., D represents a single bond, oxygen atom and the like, Rx represents a saturated alkyl group having 3 to 8 carbon atoms and the like, AR represents a partially unsaturated or completely unsaturated condensed bicyclic carbon ring or a heterocyclic ring, and Y represents hydrogen atom, a lower alkyl group having 1 to 4 carbon atoms and the like] or a salt thereof. A compound having prostaglandin production-suppressing action and leukotriene production-suppressing action is provided.

Via its info storing and processing functions (ISP), one side or both sides of the annulation and its matched handset (MH) can be used to keep the secret key or other important info. MH may become the complementary or unique device to control the annulation and the on/off of its ISP. When the annulation and its ISP are on, ISP of MH can control the working state of the info managing system of MH depending on the distance of wireless connection with MH. Wearing on the wrist, this annulations and its MH are not easy to drop but easy to use.

The invention discloses an organic compound which has a structural formula as shown in a formula (1). In the formula (1), R1 is selected from CN, CF3 and NO2; m is an integer from 0 to 2, and n is aninteger from 2 to (5-m); Ar1 is selected from hydrogen, halogen, C1-C8 alkyl, C5-C10 cycloalkyl, C1-C8 alkoxy, C6-C14 aryl and C3-C12 heteroaryl, and multiple Ar1s can be the same or different; Ar2 has a structural formula as shown in a formula (2), and multiple Ar2s can be the same or different; in the formula (2), X is selected from single bonds, O, S, NR8 and CR9R10; * denotes the position of connection between the Ar2 and a benzene ring in the formula (1); each of R2-R7 is independently selected from hydrogen or C1-C14 electron donating group, and at least one is C3-C12 non-tertiary-carbonbranched alkyl; any two of the R2-R7 can form a ring; and each of R8-R10 is independently selected from hydrogen, halogen, carbonyl, C1-C8 alkyl, C5-C10 cycloalkyl, C1-C8 alkoxy, C6-C14 aryl and C3-C12 heteroaryl or a combination thereof.

A compound of the formula:

wherein R¹ is a 5- or 6-membered ring;

• • Z¹ is a 5- or 6-membered aromatic ring;
  • Z² is a group -Z^2a-W²-Z^2b-, wherein Z^2a and Z^2b are each O, S(O)_q (wherein q is 0, 1 or 2), an imino group, or a bond; and W² is an alkylene chain;

W is a group represented by

wherein R³ and R^3′ are each a hydrogen atom, a lower alkyl group, or a lower alkoxy group; X is CH or N; n and n′ are each an integer of 0 or 1 to 4; m and m′ are each 1 or 2; Y is O, S(O)_p (wherein p is 0, 1 or 2), CH₂ or NR⁴ (wherein R⁴ is a hydrogen atom, a lower alkyl group, or a lower acyl group); and

R² is (1) an amino group, in which the nitrogen atom may be converted to a quaternary ammonium or an oxide, or (2) a nitrogen-containing heterocyclic group which may contain a sulfur atom or an oxygen atom as the ring-constituting atom, in which the nitrogen atom may be converted to a quaternary ammonium or an oxide; or a salt thereof. The compound exhibits excellent CCR antagonist activity against CCR5, and is useful as a prophylactic and/or therapeutic agent for HIV infection in human peripheral blood mononuclear cells, especially for AIDS.

Enantiomeric bicyclic lactone compounds as can be prepared via an N-heterocyclic carbene-catalyzed annulation reaction.

The present invention disclosed herein is a novel commercially feasible, one pot synthesis of library of 3-substituted phthalides of formula I via CuCN mediated oxidative cyclization in high yield. Formula I

The invention discloses a method for preparing a N-sulfonyl-1,4-oxazine derivative, in an organic solvent, tetracarboxylic rhodium is taken as a catalyst, a 1-sulfonyl-1,2,3-triazole compound and an epoxy compound are taken as substrates, so that the N-sulfonyl-1,4-oxazine derivative can be obtained. According to the invention, the N-sulfonyl-1,2,3-triazole compound and the epoxy compound are taken as the substrates for nitrogen removal and annulations reactions, so that N-sulfonyl-1,4-oxazine derivative can be obtained. The reaction raw materials have the advantages of simple preparation method, easy preservation, little rhodium catalyst usage, and greatly cost reduction. The method can be used for synthesizing a series of the N-sulfonyl-1,4-oxazine derivative, and the synthesized products have biological activity.

The invention relates to a preparation method of an allyl chlorooxyl cephalosporin compound, and belongs to the technical field of pharmaceutical synthesis. In order to solve the technical problem that an existing process is long in line and low in product yield and purity, the invention provides the preparation method of the allyl chlorooxyl cephalosporin compound. The method comprises the following steps of: performing an additive reaction on an allyl compound and chlorine to obtain a reaction liquid of a dichloro product; then, adding organic alkali for elimination reaction to obtain a compound shown as a formula III; then, performing a hydrolysis reaction of the compound shown as the formula III in a mixed solvent including dimethyl sulfoxide and water under the catalytic effect of an acidic catalyst and Cu2O to obtain an allyl alcohol intermediate; then, performing annulation under the effect of boron trifluoride diethyl etherate or methanesulfonic acid to obtain a compound shown as a formula V; and then, under the effect of an initiator, performing chlorination of the compound shown as the formula V and a chlorinating agent to obtain the allyl chlorooxyl cephalosporin compound. The method has the advantages of simple process and high product purity and yield.

An organic electroluminescence device utilizes a novel combination comprising one or more biscarbazole derivative compounds as the phosphorescent host material in combination with a green phosphorescent dopant material in the light emitting region of the device, where the biscarbazole derivative compounds are represented by a formula (1A) or (1B) below; where A₁ represents a substituted or unsubstituted nitrogen-containing heterocyclic group having 1 to 30 ring carbon atoms; A₂ represents a substituted or unsubstituted aromatic hydrocarbon group having 6 to 30 ring carbon atoms, or substituted or unsubstituted nitrogen-containing heterocyclic group having 1 to 30 ring carbon atoms; X₁ and X₂ each are a linking group; Y₁ to Y₄ each represent a substituent; p and q represent an integer of 1 to 4; and r and s represent an integer of 1 to 3; and the green phosphorescent dopant material is a phosphorescent organometallic complex having a chemical structure represented by LL′L″M wherein M is a metal that forms octahedral complexes, L, L′, and L″ are equivalent or inequivalent bidentate ligands wherein each L comprises a substituted or unsubstituted phenylpyridine ligand coordinated to M through an sp² hybridized carbon and N; and, one of L, L′ and L″ is different from at least one of the other two.

The invention relates to the field of organic functional materials. The invention provides a double-condensed-ring naphthopyran photochromic compound shown as a formula I and a preparation method thereof. The preparation method comprises the following steps: 4-methoxynaphthalen-1-ylboronic acid pinacol ester reacts with 2-bromoisophthalic acid dimethyl ester under the condition of a palladium catalyst to obtain 2-(4-methoxynaphthalen-1-yl)isophthalic acid dimethyl ester M1; the M1 and methylmagnesium bromide are subjected to addition, acidification cyclization and demethylation reactions to obtain 1,1,5,5-tetramethyl-1,5-dihydrobenzo[mno]aceanthrylene-9-ol M4; and then the compound M4 and 1,1-diaryl-2-propyn-1-ol react to generate the target compound I under acid catalysis. The compound Ican be changed from colorless to purple or blue under ultraviolet irradiation, the process is reversible, and the compound I has the characteristics of quick light response, excellent fatigue resistance, high color rate and the like. In the formula I, R<1> and R<2> are the same or different and separately represent hydrogen, straight-chain or branched-chain alkyl containing 1-6 carbon atoms, straight-chain or branched-chain alkoxy containing 1-6 carbon atoms, aryl, halogens, NH2 and -NRR.

The invention discloses camphoryl pyrimidines, and a preparation method and an anti-tumor activity study thereof. With camphor as a raw material and under an alkaline catalysis condition, a series ofalpha,beta-unsaturated ketones are obtained through aldol condensation reaction of camphor with different aromatic aldehydes respectively, a series of camphoryl pyrimidines are obtained through annulation reaction of alpha,beta-unsaturated ketones with guanidine hydrochloride through catalysis of potassium tert-butoxide, and the anti-tumor activity of the synthesized camphoryl pyrimidines is studied. Experiments show that the camphoryl pyrimidines have good inhibitory activity on human multiple myeloma cells (RPMI-8226), human breast cancer cells (MDA-MB-231) and human non-small cell lung cancer cells (A549), have less toxicity on normal cell human gastric mucosa cells (GES-1), and have potential anti-tumor application value.

The invention relates to a method for manufacturing a section of a xenophysogobio boulengeri otolith for fish age determination. The otolith of xenophysogobio boulengeri is picked, soaked, fixed, baked, cooled, grinded, degummed and mounted, clear annulations appear on the otolith of the xenophysogobio boulengeri, and therefore the age of the xenophysogobio boulengeri is determined. The new method is provided for fish age study, and is suitable for the study of the age of teleostean with two sides of the otoliths thick.

The invention belongs to the technical field of molecular materials and discloses a preparation method and application of a condensed ring furan-based small-molecular material. The method comprises the following steps: by taking 2,3-dibromofuran, 2,3-dibromothiophene, 2,3-dibromoselenophene, 2,3-dibromo-indol derivatives and 2-hydroxybenzeneboronic acid derivatives as raw materials, performing Suzuki reaction to obtain a key intermediate; by taking cuprous or a copper compound as a catalyst, and 1,10-phenanthroline or dipyridyl compound as a ligand, generating intramolecular Ullmann C-O coupling reaction, and synthesizing a series of condensed ring furan small-molecular materials. The substrate is relatively simple to synthesize and high in yield; the ring forming reaction time of furan is greatly shortened; the cuprous compound or dipyridyl compound as a catalyst system are cheap; the reaction conditions are milder; the application range of the substrate is wide; the reaction yield is high up to 97%. Therefore, the method is suitable for industrial production.

A compound is represented by the following formula (1). In the formula (1), Ar is a substituted or unsubstituted aryl group including 6 to 30 ring carbon atoms, R^a are independently a substituted or unsubstituted alkyl group including 1 to 15 carbon atoms, or a substituted or unsubstituted cycloalkyl group including 3 to 15 carbon atoms, R^b1 to R^b4 are independently a halogen atom, a cyano group, a substituted or unsubstituted alkyl group including 1 to 15 carbon atoms, or the like, R^c1 to R^c10 are independently a hydrogen atom, a halogen atom, a cyano group, a substituted or unsubstituted alkyl group including 1 to 15 carbon atoms, or the like, * is a bonding position at which one of R^c1 to R^c10 is bonded to either nitrogen atom, x is an integer from 0 to 3, y is an integer from 0 to 4, and z are independently an integer from 0 to 5.

The invention discloses a fluorine-containing three-membered ring compound shown in the formula V-a, V-b or V-c and a preparation method thereof. The preparation method comprises that in an organic solvent, fluoroalkyl sulfur ylide shown in the formula III' and a double-bond compound shown in the formula IV-a, IV-b or IV-c undergo an annulation reaction to produce the fluorine-containing three-membered ring compound shown in the formula V-a, V-b or V-c. The invention also discloses a preparation method of a fluoroalkyl sulfonium salt shown in the formula III or IV. The preparation method comprises that sulfur ether shown in the formula I and fluoroalkyl sulfonate shown in the formula II or a compound shown in the formula II' undergo a nucleophilic substitution reaction in a solvent or without a solvent. The preparation method has simple processes, utilizes easily available raw materials, has short reaction time, a high product yield, high product purity, mild conditions and simple and convenient post-treatment processes and can be industrialized easily.