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序号 专利名 申请号 申请日 公开(公告)号 公开(公告)日 发明人
401 Production of levulinic acid JP29254189 1989-11-13 JPH02202846A 1990-08-10 BERUNAARU KAPE; GI RARUTEIGOO
PURPOSE: To easily obtain highly pure and essentially colorless levulinic acid by progressively introducing furfuryl alcohol to a mixture of water as a reaction solvent, strong protonic acid and levulinic acid, and then heating. CONSTITUTION: In the presence of water and a strong protonic acid not acidified under reaction conditions (i.e., protonic acid with an acidity constant Ho lower than -4), furfuryl alcohol is heated to prepare levulinic acid. Furfuryl alcohol is progressively introduced to a mixture of water as a reaction solvent, strong protonic-acid and levulinic acid, for a few minutes to tens of hours, preferably, for 1-12 hours. Here, 1 to 25 mol, preferably, 1.5 to 10 mol of water is used for 1 mol of furfuryl alcohol, 30-100 wt.%, preferably, 50 to 500 wt.% of levulinic acid as a solvent for the whole furfuryl alcohol, and 1 to 50 wt.%, preferably, 2 to 20 wt.% of strong protonic acid for the water. COPYRIGHT: (C)1990,JPO
402 Production of cis-propanecarboxylic acid JP10033389 1989-04-21 JPH029838A 1990-01-12 ARAN KURIFU
PURPOSE: To obtain the title compd. of high purity by treating a compd. obtained by esterifying a novel compd. such as 4-hydroxy3,3,6,6-tetrabicyclo [3.1.0] hexan-2-one with a hydroxyl ion supply source in an aq. medium. CONSTITUTION: A compd. represented by formula I (wherein R is an atom or a group capable of forming an anion R - stable under a reaction condition, especially pref., hydroxy, sulfonyloxy and methanesulfonyloxy and R 1 and R 2 are H or methyl) is treated with a hydroxyl ion supply source (especially pref., alkali metal hydroxide) in an aq. medium (especially pref. containing an aprotic solvent) to obtain cis-cyclopropanecarboxylic acid. The compd. represented by the formula I is obtained by esterifying a novel compd. represented by formula III. The compd. represented by the formula III is obtained by treating a novel compd. represented by formula IV with a reducing agent. This method does not produce a trans isomer in parallel and is advantageous. COPYRIGHT: (C)1990,JPO
403 Preparation of 3-(2-chloro-2-(4-chlorophenyl)-vinyl)-2,2-dimethylcyclopropanecarboxylic acid JP32807888 1988-12-27 JPH01203350A 1989-08-16 RAINHARUTO RANCHIYU
PURPOSE: To economically obtain the compound in high yield by allowing 3- chloro-3-(4-chlorophenyl)-propenal to react with chloromethyl isopropyl ketone without isolation of the product and allowing the product to react with an aqueous base. CONSTITUTION: In a first step, 4,4-dimethyl-1,3,6-trichloro-1-(4-chlorophenyl)-hex-1- en-5-one is obtained by allowing 3-chloro-3-(4-chlorophenyl)-propenal to react with preferably approximately equilmolar chloromethyl isopropyl ketone or up to 4 equivalents of it if diluents are not used. In a second step, the objective compound is obtained by allowing the product without isolation to react with an aqueous bases or an alkoxide usually at the room temperature. COPYRIGHT: (C)1989,JPO
404 JPS6360115B2 - JP12345985 1985-06-06 JPS6360115B2 1988-11-22
405 Production of tetrafluorophthalic acid JP17888287 1987-07-20 JPS63258442A 1988-10-25 HARUAKI ITO; NOBUO ISHIKAWA; UTARO MATSUSHITA; MASAAKI SHIMIZU; TOSHIAKI SHIMIZU
PURPOSE: To obtain the titled compound useful as a synthetic intermediate for pharmaceuticals, agricultural chemicals and other industrial products, in high yield in two steps, by reacting an imide with an alkali metal fluoride and hydrolyzing the reaction product. CONSTITUTION: An imide of formula I or formula II (R 1 is univalent hydrocarbon group or heterocyclic group; R 2 is bivalent hydrocarbon group or heterocyclic group; X 1WX 4 are Cl or Br) is made to react with an alkali metal fluoride. The reaction is carried out preferably in the presence of a catalyst (e.g. quaternary ammonium salt) in a solvent (e.g. N,N-dimethylformamide) or in the absence of solvent at 80W220°C to obtain the corresponding N-substituted- tetrafluorophthalimide or diimide. The objective compound is produced by hydrolyzing the imide or diimide at 70°CWrefluxing temperature using sulfuric acid, etc. The alkali metal fluoride is e.g. potassium fluoride. COPYRIGHT: (C)1988,JPO&Japio
406 Manufacture of cinnamic acid JP858088 1988-01-20 JPS63198643A 1988-08-17 GABURIERE IIRU; GIYUNTERU ROTSUSHIERU; NORUBERUTO MAIERU
407 Stereoconvergent process for producing optically active carboxylic acid JP32417387 1987-12-23 JPS63190851A 1988-08-08 MARUKO BUIRA; KURAUDEIO JIYORUDAANO; GURAJIAANO KASUTARUDEI; SHIRUBUIA KABUITSUCHIOORI
408 JPS63501720A - JP50000487 1986-11-25 JPS63501720A 1988-07-14
A ring contraction approach is applied to preparation of cyclopentane derivatives, especially 2,2,5,5-tetra-methylcyclopentanecarboxylic acid from cyclohexane compounds. In one aspect, a cyclohexane diazoketone is reacted with an amine (e.g., an alanine ester) to form the corresponding cyclopentane acid amide.
409 Synthesis of carboxylic acid JP19053787 1987-07-31 JPS6341439A 1988-02-22 KURAUDEIO JIYORUDAANO; MARUKO BUITSURA
410 Manufacture of optically active carboxylic acid and related intermediates JP17897186 1986-07-31 JPS6277378A 1987-04-09 KURAUDEIO JIYORUDAANO; GURAJIAANO KASUTARUDEI
411 Intermediate for synthesizing carboxylic acid JP17897286 1986-07-31 JPS6229582A 1987-02-07 KURAUDEIO JIYORUDAANO; GURAJIAANO KASUTARUDEI
412 Manufacture of alpha-hydroxy acid JP27058285 1985-11-29 JPS61191649A 1986-08-26 JIYAN DANIERU ANDORE; PIEERU JIYAN GUROTSUSHI; ARAN EIMU; JIYOBANNI BENERUTSUCHI MANZARO
The invention relates to a process for preparing alpha -hydroxy-acids of general formula: in which R represents hydrogen or a lower alkyl radical and Cy represents a phenyl, naphthyl or heterocyclic radical, these latter three radicals optionally comprising one or more substituents selected from the group consisting of lower alkyl, lower alkenyl, lower alkynyl, lower alkoxy radicals and halogen atoms, process which comprises the treatment of an alpha -monohalogenated ketone of general formula: in which R and Cy have the same meaning as above and X represents chlorine, bromine or iodine, in the presence of an aqueous solution of an alkali metal hydroxide, a non-polar organic solvent selected from an aromatic or alicyclic hydrocarbon and oxygen in excess optionally in the presence of an inert gas, the treatment being carried out at a temperature ranging from the boiling temperature of the reaction medium at atmospheric pressure and 240 DEG C. under pressure and the alkali metal so formed is then acidified to obtain the desired acid.
413 Manufacture of optically active alpha-arylalkanoic acid and novel intermediate JP7338885 1985-04-06 JPS60228441A 1985-11-13 KURAUDEIO GIORUDANO; GURAJIANO KASUTARUDEI; FURUBIO UGERI; SHIRUBIA KABITSUCHIORI
414 Manufacture of optically active alpha-arylalkanoic acid JP3625985 1985-02-25 JPS60208941A 1985-10-21 GURAJIANO KASUTARUDEI; KURAUDEIO JIYORUDAANO; FURUBIO UTSUGERI
415 Manufacture of alpha-arylalkanoic acid JP1982685 1985-02-04 JPS60199851A 1985-10-09 FURUBIO UTSUGERI; GURAJIANO KASUTARUDEI; KURAUDEIO JIYORUDAANO
416 Tetrahydropyridazinone derivative, manufacture and use JP12460284 1984-06-19 JPS6013766A 1985-01-24 GERUHARUTO TSUOORERU; RUUDEI BAIERURE; MERITA YUSUTO; PIERO MARUTORANA; HERUMUUTO BOON; RORUFUUEEBERUHARUTO NITSUTSU
417 JPS5932455B2 - JP16170379 1979-12-14 JPS5932455B2 1984-08-09 JON GUREI DEINGUOORU; HANSU GUROITAA; PIEERU MARUTEIN; PEETAA ATSUKAAMAN; ROORENTSU GUZEERU
There is described a new process for the preparation of optically active 2-(2',2'-dihalogenovinyl)-cyclopropane-1-carboxylic acids substituted in the 3 position, and derivatives thereof. A racemate of certain cyclobutanones is reacted with a sulfurous acid salt of an optically active base to obtain a mixture of diastereomeric 4-(2',2',2'-trihalogenoethyl)-cyclobutane-2-sulfonic acid salts; this mixture is then separated into the pure diastereomeric sulfonic acid salts. Either the pure diastereomeric sulfonic acid salts are converted directly to the desired optically active products, or the optically active cyclobutanones obtained from the pure diastereomeric sulfonic acids salts by decomposition are converted, in the presence of a base, to the desired product. Optionally, the product, optically active 2-(2',2'-dihalogenovinyl)-cyclopropane-2-carboxylic acids can be converted to their 1',2'-dibromo derivatives.
418 Manufacture of arylalkanoic acid ester JP20570183 1983-10-31 JPS59104347A 1984-06-16 KURAUDEIO GIORUDAANO; GURACHIANO KASUTARUDEI
419 Preparation of 1-oxacephem compound JP14726882 1982-08-24 JPS5936684A 1984-02-28 YAMAMOTO SADAO; ITANI HIKARI; TAKAHASHI HIROMI; TSUJI SHIYOUJI; NAGATA WATARU
NEW MATERIAL:A compound shown by the formula I [R is carboxy-protecting group; R 1 is (substituted)alkyl, aralkyl, or allyl; X is oxo, or (substituted)methylene; with the proviso that double bond =X may be transferred into the ring to form 3-cephem ring]. EXAMPLE: 7α-Benzamido-3-methylene-1-dethia-1-oxacephem-4α-carboxylic ester. USE: An intermediate for synthesizing 1-oxacephem antibacterial antibiotic, etc. PROCESS: For example, an oxazolinoazetidinone compound shown by the formula II(Z is H, or amino-protecting group) is reacted with diazobutyric ester compound shown by the formula III (Y is halogen, or hydroxy), and, if necessary, the amino-protecting group is removed to give 2-diazo-3-substituted-4-(2-oxo-3-amidoazetidin-4-yl)oxybutyric ester shown by the formula IV, which is subjected to carbenoid insertion reaction to give a compound shown by the formula I . COPYRIGHT: (C)1984,JPO&Japio
420 Preparation of 4-homoisotwistane-3-carboxylic acid JP12823482 1982-07-22 JPS5920244A 1984-02-01 FUJIKURA YOSHIAKI; TAKAISHI NAOTAKE; INAMOTO YOSHIAKI
PURPOSE: To prepare the titled compound useful as an intermediate of a compound having antiviral activity, extremely easily, without loss, in high purity and yield, reducing the consumption of acid, by using a formic acid ester as a starting substance, and contacting the substance with a strongly acidic inorganic catalyst. CONSTITUTION: The objective compound of formula II is prepared by using tricyclo[5,2,1,0 2, 6]dec-8-yl-methyl formate of formula I as a starting substance, and reacting the substance in the presence of a strongly acidic inorganic catalyst preferably at 0W80°C. The strongly acidic inorganic catalyst is e.g. concentrated sulfuric acid, phosphoric acid, hydrofluoric acid, boron trifluoride-phosphoric acid, etc., and its amount is preferably 0.5W24mol, especially ≤6mol for concentrated sulfuric acid per 1mol of the compound of formula I . The starting compound of formula I can be prepared either by mixing and reacting an alcohol compound with formic acid, or by reacting the mixture in the presence of a small amount of concentrated sulfuric acid, arylsulfonic acid, etc. COPYRIGHT: (C)1984,JPO&Japio
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