- One-pot method for preparing diepoxide (by machine translation)
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The method comprises the following steps, adding a reducing agent water solution :S1. to a reactor: slowly dropwise adding a reducing agent aqueous solution to obtain the diepoxide, adding a reducing agent aqueous solution to the reactor, to obtain the diepoxy, and separating and purifying ;S2. from the organic phase: by one-pot reaction, and adding a reducing agent water, through a pot method to obtain the diepoxide crude solution, to obtain the diepoxide compound. The invention discloses a method for separating and purifying a diepoxide crude product through a high vacuum, distillation . The method comprises the following steps of: adding a reducing agent aqueous solution to the, reactor at a low temperature, to obtain a diepoxide 91% crude, product through 95% a, one-pot reaction, of the diolefin and the m-chloroperoxybenzoic acid solution to obtain a diepoxide crude product solution. (by machine translation)
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Page/Page column 6-9
(2020/05/01)
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- Method for preparing m-chloroperoxybenzoic acid by utilizing phase transfer catalysis
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The invention discloses a method for preparing m-chloroperoxybenzoic acid by utilizing phase transfer catalysis. The method comprises the following steps: dissolving m-chlorobenzoic acid in an organicsolvent, adding an aqueous acidic oxidant solution with a pH value of 1-4, carrying out an oxidation reaction under the action of a phase transfer catalyst, carrying out extraction separation to obtain an organic phase, drying, and separating out filter residues to obtain an organic solution containing m-chloroperoxybenzoic acid. The m-chloroperoxybenzoic acid is obtained by catalyzing the reaction of m-chlorobenzoic acid and an oxidant through the phase transfer catalyst, the raw materials are stable in properties, cheap and easy to obtain, the process is simple and easy to control, the solvent can be recycled, the product yield is high, the yield of the m-chloroperoxybenzoic acid can reach 82% or above, and large-scale industrial production is facilitated.
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Paragraph 0026-0033
(2020/05/02)
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- Synthetic method for drug intermediate m-chloroperbenzoic acid
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The invention discloses a synthetic method for the drug intermediate m-chloroperbenzoic acid. The synthetic method comprises the following steps: adding m-chlorophenylacetamide and a sodium nitrate solution into a reaction vessel, controlling a stirring speed to be 230-260 rpm and a solution temperature to be 10-16 DEG C, adding a methyl n-butyl ether solution and a 1,4-butanediol solution, addingN-bromoacetamide in batches within 20-40 min, and continuing a reaction for 60-90 min; and then adding an aqueous solution and zinc fluoride powder, controlling a stirring speed to be 310-330 rpm, continue the reaction for 3-4 h, carrying out washing with a sodium chloride solution for 30-50 min, then carrying out washing with a 3-heptanol solution for 20-40 min, carrying out recrystallization ina nitroethane solution, and then carrying out dehydration with a dehydrating agent so as to obtain the finished m-chloroperoxybenzoic acid.
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Paragraph 0016-0019; 0020-0023; 0024-0027
(2018/07/30)
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- Copper Tetrasulfophthalocyanine Intercalated Hydrotalcite as an Efficient Bifunctional Catalyst for the Baeyer–Villiger Oxidation
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Abstract: A heterogeneous bifunctional hybrid catalyst originated from copper tetrasulfophthalocyanine (CuPcTs) and hydrotalcite for Baeyer–Villiger (B-V) oxidation has been prepared and characterized. XRD, FTIR, DR UV-Vis and SEM characterization indicate that CuPcTs molecule has been successfully intercalated into the layer of ZnAl hydrotalcite. And the synthesized hybrid exhibited excellent catalytic activity in the B-V oxidation for various ketones under mild conditions. Its bifunctional role in the reaction through O2/benzaldehyde has been discussed and verified by controlled experiments. The study indicates that the designed catalyst not only catalyzes the oxidation of benzaldehyde to perbenzoic acid, but also accelerates the transformation of ketone to lactone or ester. Graphical Abstract: [Figure not available: see fulltext.]
- Zhou, Weiyou,Chen, Yong,Qian, Junfeng,Sun, Fu’an,He, Mingyang,Chen, Qun
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p. 2157 - 2164
(2016/10/18)
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- METHOD FOR PRODUCING AMIDE COMPOUND
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Disclosed is a method for producing an amide compound represented by the formula (3) below and having an excellent control activity against a harmful arthropod, which is characterized in that an aniline compound represented by the formula (1) below and an aldehyde compound represented by the formula (2) below are reacted in a solvent in the presence of an oxidizing agent such as oxygen or a peroxide. (In the formulae below, R1, R2 and R3 independently represent a C1-C6 alkyl group which may be substituted by a halogen atom, or the like; and R4, R5, R6 and R7 independently represent a halogen atom or the like.)
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Page/Page column 25; 27
(2010/01/29)
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- TRICYCLIC COMPOUNDS HAVING ACTIVITY AS Ras-FPT INHIBITORS
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Compounds of formula (I), wherein: X is hydrogen, halogen, CF3, nitro, NH2 or lower alkyl; each X is independently selected from the group consisting of hydrogen, halogen, lower alkoxy and lower alkyl; n is 1 or 2; Y is selected from the group consisting of S(O)p, O, and NR, wherein p is 0, 1 or 2, and R is hydrogen, alkyl, aryl, cycloalkyl, loweralkoxycarbonyl, aminocarbonyl or acyl; R and R, which may be the same or different, are selected from the group consisting of hydrogen and lower alkyl groups, or taken together can form an oxygen atom when Y is NR; A..... is C=, CH- or N-; R is -CZ-Y-Y-R, wherein: Z is O, =CH-CN, or =N-CN; one of Y and Y is a bond, -CO-, O, S, or -NR-, and the other is (CH2)m, where m is 0 or an integer of 1 to 4, and R is H or alkyl, with the previso that when Z is O and m is 0 then Y or Y is selected form -CO-, O, S, or -NR; R is aryl, heteroaryl or heterocycloalkyl, with proviso that R can also be lower alkyl when Z is =N-CN; and their pharmaceutically acceptable acid additions salts; have activity as Ras-FPT inhibitors. They can be used, e.g., in pharmaceutical compositions, for inhibiting the abnormal growth of cells and for inhibiting proliferative diseases. Processes for their preparation, and useful intermediates, are also disclosed.
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- Pyrazinone thrombin inhibitors
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Compounds of the invention are useful in inhibiting thrombin and associated thrombotic occlusions having the following structure: or a pharmaceutically acceptable salt thereof, wherein A is
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- Steroids as neurochemical stimulators of the VNO to treat paroxistic tachycardia
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The invention relates to a method of alleviating the symptoms of PMS and anxiety. The method comprises nasally administering a steroid which is a human vomeropherin, such that the vomeropherin binds to a specific neuroepithelial receptor. The steroid or steroids is/are preferably administered in the form of a pharmaceutical composition containing one or more pharmaceutically acceptable carriers.
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- Tricyclic compounds having activity as RAS-FPT inhibitors
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Compounds of Formula I: wherein: X1 is hydrogen, halogen, CF3, nitro, NH2 or lower alkyl; each X2 is independently selected from the group consisting of hydrogen, halogen, lower alkoxy and lower alkyl; n is 1 or 2; Y is selected from the group consisting of S(O)p, O, and NR5, wherein p is 0, 1 or 2, and R5 is hydrogen, alkyl, aryl, cycloalkyl, loweralkoxycarbonyl, aminocarbonyl or acyl; R1 and R2, which may be the same or different, are selected from the group consisting of hydrogen and lower alkyl groups, or taken together can form an oxygen atom when Y is NR5; A . . . is C=, CH- or N-; R is -CZ-Y1-Y2-R3, wherein: Z is O, =CH-CN, or =N-CN; one of Y1 and Y2 is a bond, -CO-, O, S, or -NR4-, and the other is (CH2)m, where m is 0 or an integer of 1 to 4, and R4 is H or alkyl, with the proviso that when Z is O and m is 0 then Y1 or Y2 is selected from -CO-, O, S, or -NR4; R3 is aryl, heteroaryl or heterocycloalkyl, with the proviso that R3 can also be lower alkyl when Z is =N-CN; and their pharmaceutically acceptable acid addition salts; have activity as Ras-FPT inhibitors. They can be used, e.g., in pharmaceutical compositions, for inhibiting the abnormal growth of cells and for inhibiting proliferative diseases. Processes for their preparation, and useful intermediates, are also disclosed.
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- Pyrimidine derivatives and guanine derivatives, and their use in treating tumor cells
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The present invention provides certain 6-hetarylalkyloxy pyrimidine derivatives of formula II wherein R is (i) a cyclic group having at least one 5- or 6-membered heterocyclic ring, optionally with a carbocyclic or heterocyclic ring fused thereto, the or each heterocyclic ring having at least one hetero atom chosen from O, N, or S, or a substituted derivative thereof; or (ii) phenyl or a substituted derivative thereof, R2 is selected from H, C1-C5 alkyl, halogen or NH2, R4 and R5 which are the same or different are selected from H, NH2 or NOn where n=1 or 2, or R4 and R5 together with the pyrimidine ring form a 5- or 6-membered ring structure containing one or more heterocyclic atoms, and pharmaceutically acceptable salts thereof, exhibit the ability to deplete O6-alkylguanine-DNA alkyltransferase (ATase) activity.
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- Preparation of 14-hydroxynormorphinones from normorphinone dienol acylates
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The invention provides processes for the conversion of normorphinone and its derivatives, which can be synthesized from morphine, to the corresponding 14-hydroxynormorphinone and its derivatives including oxycodone, oxymorphone, noroxymorphone and naltrexone. Noroxymorphone is a key intermediate for the production of important narcotic analgesics and antagonists. The invention also provides certain novel intermediates.
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- Glycoprotein IIb/IIIa antagonists
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This invention relates to certain bicyclic compounds having a nucleus formed of two fused six membered rings, for example, benzopyran, isoquinoline, isoquinolone, tetrahydronaphthalene, dihydronaphthalene, or tetralone, substituted with both basic and acidic functionality, which are useful in inhibition of platelet aggregation.
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- Binding compentent oligomers containing unsaturated 3',5' and 2',5' linkages
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Oligonucleotide analogs having one or more substitute linkages of the formula 2'/3'--S--CH2 --CH=5' or 2'/3'--O--CH2 --CH=5' between adjacent nucleomonomers are disclosed. The substitute linkage replace the usual phosphodiester linkage found in unmodified nucleic acids. The oligonucleotide analogs are easy to synthesize, stable in vivo, resistant to endogenous nucleases and are able to hybridize to target nucleic acid sequences in a sequence specific manner.
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- Bicyclic nucleosides, oligonucleotides, process for their preparation and intermediates
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Compounds of the formula I in the form of the racemates or enantiomers thereof, STR1 in which R1 and R2 independently of one another are hydrogen or a protective group, and B is a purine or pyrimidine radical or an analogue thereof, can be used as antiviral active ingredients or for the preparation of biologically active oligonucleotides.
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- Mitomycin derivatives
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Novel mitomycin derivatives are characterized by a substituent on the C6 -methyl group. The mitomycin derivatives exhibit anti-tumor and antibacterial activity and have low toxicity.
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- α-Hydroxy thioethers
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Novel asymmetric thioethers of the formula STR1 in which the general symbols have the following meanings: a is an integer of from 1 to 7, Ro represents hydrogen or C1-7 -alkanoyl, R1 represents C1-3 -alkyl which may be substituted at the terminal carbon atom by a free or acylated hydroxy group, by a halogen atom having an atomic number of at most 17, or by methoxy, or represents C1-3 -perfluoroalkyl, R2 represents an optionally unsaturated aliphatic radical having from 5 to 15 carbon atoms, A represents ethylene or alternatively, if R1 represents a halogenated radical and/or B represents phenylene or ethylene, a single bond or vinylene, B represents a single bond, ethynylene or phenylene, R3 represents hydroxy, C1-7 -alkoxy or an optionally substituted amino group, and --X-- represents a single bond, a methylene group of an optionally N-acylated primary aminomethylene group, and their salts are active as leucotriene antagonists since they eliminate the contractions of smooth muscles brought about by leucotrienes, and are therefore suitable for the treatment of allergic, especially asthmatic, conditions.
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- POLYMER-SUPPORTED PERSULFONIC ACID AS OXIDISING AGENT
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A polymer-supported persulfonic acid has been prepared and applied for the oxidation of carboxylic acids, ketones, olefins, and disulfide bonds of cystine and cystinyl peptides to their peracids, esters (lactones), epoxides and sulfonic acid derivatives respectively in good yields.The resin also effectively removed the formyl protection from formyl amino acids.Spent polymer was reactivated by simple reactions.
- Pande, C. S.,Jain, N.
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p. 1271 - 1280
(2007/10/02)
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- Dianhydrohexite derivatives, and their use as pharmaceuticals
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Dianhydrohexites of the formula STR1 wherein R1 is hydrogen or benzyl, R2 is alkyl or omega-theophyllin-7-yl-alkyl, and R1 and R2 together with the nitrogen atom to which they are attached form a bicyclic group and R3 is hydrogen, acyl, pyridylcarbonyl, nitro or a hydroxylamino group, are formed by an analogous method and used as pharmaceuticals in the treatment of heart and circulatory diseases.
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- PHASE TRANSFER CATALYSED PEROXIDATION OF CARBOXYLIC ACIDS WITH POTASSIUM PERSULFATE
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Aqueous solution of potassium persulfate converts water-insoluble carboxylic acids in ether (or dichloromethane), to peracids in a yield of 80-90percent under the catalytic influence of benzyltriethylammonium chloride (BTEAC) or polyethyleneglycol (PEG-400).The reaction is further catalyzed kinetically in presence of a sulfonated polymer.
- Pande, C. S.,Jain, Neena
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p. 2123 - 2128
(2007/10/02)
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- INFLUENCE OF CERTAIN PARAMETERS ON SYNTHESIS OF m-CHLOROPERBENZOIC ACID.
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m-Chloroperbenzoic acid (m-CPBA), which is a promising intermediate for production of bleaching agents, is prepared by the reaction of m-chlorobenzoyl chloride (m-CBC) with 30% hydrogen peroxide in aqueous alcohol in presence of potassium hydroxide and a stabilizer, followed by isolation of the peroxy acid by acidification of a solution of its salt and extraction with chloroform. The pupose of this work was to investigate the influence of the principal synthesis parameters on the yield and quality of the reaction product. The effects of parameters such as solvent-water ratio, CBC-water ratio, stirrer speed, and stabilizer concentration on the product purity were tested.
- Palei,Sorokina,Duryagina,Kolomiets
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p. 353 - 356
(2007/10/02)
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- PREPARATION OF CHLOROPERBENZOIC ACIDS.
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A method was recently proposed whereby an acyl chloride is reacted with 30% hydrogen peroxide at room temperature in aqueous alcoholic solution in presence of potassium hydroxide and a stabilizer (magnesium sulfate). The resultant solution of the salt of the peroxy acid is acidified with sulfuric acid, and the liberated acid is extracted with chloroform. The objective of this research is to examine the possibility of using this method for preparation of chloroperbenzoic acids and to study the influence of the principal synthesis parameters on the yield and quality of the products. Based on experimental results, it is found that the process can be intensified considerably by decrease of the relative amount of solvent used.
- Palei,Sorokina,Krasil'nikova,Kolomiets
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p. 1014 - 1017
(2007/10/02)
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