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公开(公告)号：JPH0649008A
公开(公告)日：1994-02-22
申请号：JP5288992
申请日：1992-03-11
Applicant: MITSUI PETROCHEMICAL IND
Inventor： KONDO MASAHIRO , TANAKA MICHIO , SAKAMOTO NAOYA , OYOSHI HAJIME
IPC: C07C227/42 , C07C227/02 , C07C227/10 , C07C229/52
Abstract: PURPOSE:To produce a keto-acid in high selectivity with suppressing by-products by selecting the amount of a solvent used so as to precipitate the formed keto- acid and to advance reaction in a slurried state in the reaction between a m- aminophenol derivative and phthalic anhydride. CONSTITUTION:A m-aminophenol derivative of formula I (R and R are 1-6C alkyl or 4-8C cycloalkyl)(e.g. N,N-diethyl-m-aminophenol) is reacted with phthalic anhydride to give a keto-acid of formula II (e.g. 4-N,N-diethylamino-2-hydroxy-2'- carboxybenzophenone). In the reaction, 0.5-3 pts.wt. reaction solvent is used based on 1 pt.wt. m-aminophenol derivative in order to precipitate the keto-acid formed by the reaction and the reaction is carried out in a slurried state. Benzene, toluene, xylene, ethers, etc., are used as the reaction solvent. Secondary crystallization can be done under pressure depending upon the amount of the keto-acid in the solvent. The high-purity keto-acid is obtained in high yield.
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公开(公告)号：JPH0597781A
公开(公告)日：1993-04-20
申请号：JP27897291
申请日：1991-10-01
Applicant: MITSUI PETROCHEMICAL IND
Inventor： OYOSHI HAJIME , KONDO MASAHIRO , TARUMOTO HIROMASA , TANAKA MICHIO
IPC: C07C213/02 , C07C215/76
Abstract: PURPOSE:To obtain the subject compound useful as an intermediate for agricultural chemicals in high selectivity and yield without causing corrosion of a reactor by reacting specific aminophenols with dialkyl sulfate under specified conditions. CONSTITUTION:Aminophenols such as o-aminophenol expressed by formula I (R is H or alkyl) are reacted with a dialkyl sulfate such as dimethyl sulfate at 30-70 deg.C to provide the objective compound of formula II (R is alkyl). Furthermore, the dialkyl sulfate is preferably used in an amount of 1.0-1.2mol, based on 1mol compound of formula I.
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公开(公告)号：JPH04341593A
公开(公告)日：1992-11-27
申请号：JP11197991
申请日：1991-05-16
Applicant: MITSUI PETROCHEMICAL IND
Inventor： TANAKA MICHIO , FUJIMOTO TADAAKI , MIKI HISAYA
IPC: C25B3/02
Abstract: PURPOSE:To provide a method for obtaining aqueous quaternary ammonium hydroxide at a high yield by electrolyzing tetramethyl ammonium hydrogen carbonate aqueous solution while suppressing the damage of electrodes or an exchange film. CONSTITUTION:Dimethyl carbonate and trimethyl amine are allowed to react in the presence of methanol to obtain a reactional mixture incorporating tetramethylammonium methyl carbonate. Water is added to the mixture, and while distillating the water, methanol, trimethyl amine, an aqueous solution incorporating essentially tetramethyl ammonium hydrogen carbonate and
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公开(公告)号：JPH04334353A
公开(公告)日：1992-11-20
申请号：JP10105091
申请日：1991-05-02
Applicant: MITSUI PETROCHEMICAL IND
Inventor： TANAKA MICHIO , FUJIMOTO TADAAKI , MIKI HISAYA
IPC: C07C209/20 , C07C211/63
Abstract: PURPOSE:To simply produce the subject compound by a short process in a short time in a good productivity by reacting dimethyl carbonate with trimethyl amine in the presence of methanol, subsequently hydrolyzing the reaction product only with water and simultaneously removing the methanol. CONSTITUTION:Dimethyl carbonate is reacted with trimethyl amine in the presence of methanol. The produced tetramethyl ammonium methyl carbonate contained in the reaction mixture is subjected to a hydrolysis reaction only with water, preferably ultrapure water, and simultaneously to a removal of the methanol to rapidly produce an aqueous solution of the tetramethyl ammonium bicarbonate. Preferably, the reaction is performed with water in a molar ratio of 1:5-100 between the tetramethyl ammonium bicarbonate and the water at 0-120 deg.C under a pressure of 10-500mmHg. The method gives aqueous solution of tetramethyl ammonium bicarbonate reduced in the amount of the remaining methanol.
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公开(公告)号：JPH0422891B2
公开(公告)日：1992-04-20
申请号：JP704284
申请日：1984-01-20
Applicant: MITSUI PETROCHEMICAL IND
Inventor： MIZUNO KENICHI , MATSUMOTO TETSUHIRO , TANAKA MICHIO
IPC: C07C29/132 , C07C27/00 , C07C29/50 , C07C33/26 , C07C67/00
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Patent Agency Ranking
公开(公告)号：JPH0234332B2
公开(公告)日：1990-08-02
申请号：JP1540083
申请日：1983-02-03
Applicant: MITSUI PETROCHEMICAL IND
Inventor： NAKAGAWA HIROAKI , TANAKA MICHIO , MIZUNO KENICHI
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公开(公告)号：JPH02115140A
公开(公告)日：1990-04-27
申请号：JP26763788
申请日：1988-10-24
Applicant: MITSUI PETROCHEMICAL IND
Inventor： KONDO MASAHIRO , TANAKA MICHIO , TANIGUCHI KATSUO
Abstract: PURPOSE:To obtain the subject compound useful as an intermediate for pharmaceuticals, agricultural chemicals, etc., with simple process in high yield at a low cost by using an aromatic compound having isopropenyl group as a raw material and oxidizing the material with oxygen in the presence of a catalyst. CONSTITUTION:The objective compound can be produced by using an aromatic compound having isopropenyl group as a raw material and oxidizing the material with oxygen (preferably air) in the presence of a catalyst. The amount of oxygen is preferably reaction equivalent or more. The catalyst is preferably produced by supporting a transition metal (e.g., chromium, copper or manganese) on a carrier in the form of a compound or ion. Especially preferably, the catalyst is a lamellar clay mineral subjected to ion-exchange with a transition metal ion. The reaction is carried out preferably by charging the raw material, catalyst and solvent in a reaction vessel, introducing oxygen into the vessel under pressure while stirring the content and oxidizing the raw material at 100-200 deg.C (preferably 120-160 deg.C) under 5-50kg/cm pressure.
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公开(公告)号：JPH02115139A
公开(公告)日：1990-04-27
申请号：JP26588288
申请日：1988-10-21
Applicant: MITSUI PETROCHEMICAL IND
Inventor： TANAKA MICHIO , ISHIBASHI MASAYASU , TANIGUCHI KATSUO
Abstract: PURPOSE:To obtain the subject compound useful as a raw material for liquid crystal, liquid crystal polymer, etc., in high yield on an industrial scale at a low cost by using easily available cyclohexylhydroquinones as raw materials. CONSTITUTION:The objective compound of formula II can be produced by the dehydrogenation reaction of cyclohexylhydroquinones of formula I (R1 is H or hydrocarbon group) in the presence of a dehydrogenation catalyst and preferably a hydrogen acceptor such as phenol at 200-350 deg.C (preferably 250-330 deg.C) usually for 1-6hr (preferably 2-4hr). The dehydrogenation catalyst is e.g., Raney nickel, palladium black, etc., and its amount is usually 0.0005-2g-atom (preferably 0.001-0.1g-atom) in terms of metal atom based on 1mol of the compound of formula I. The starting compound of formula I can be synthesized by reacting hydroquinone with cyclohexanols in the presence of a catalyst.
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公开(公告)号：JPH01102037A
公开(公告)日：1989-04-19
申请号：JP26127287
申请日：1987-10-15
Applicant: MITSUI PETROCHEMICAL IND
Inventor： TANAKA MICHIO , KURANO YOSHITO , TANIGUCHI KATSUO
Abstract: PURPOSE:To simply obtain the titled compound, by carrying out redox reaction between 2,6-di-t-butylphenol and 3,3',5,5'-tetra-t-butyl-4,4'-diphenoquinone and dealkylation reaction of the reaction product under a specific condition at one stage. CONSTITUTION:Synthetic reaction of (C) 3,3',5,5'-tetra-t-butyl-4,4'-dihydroxybi phenyl from (A) 2,6-di-t-butylphenol and (B) 3,3',5,5'-tetra-t-butyl-4,4'- diphenoquinone by redox reaction and formation reaction of the titled compound by dealkylation of the reaction product are carried out in the presence of an acid catalyst and a solvent, preferably a phenol, diphenyl ether, sulfolane, paraf fin or gas oil at 20-280 deg.C at one stage to obtain the titled compound useful as an oxidation stabilizer for resins directly from the above-mentioned raw materials A and B or further C at one stage without separating the intermediate C.
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公开(公告)号：JPS6490147A
公开(公告)日：1989-04-06
申请号：JP24631787
申请日：1987-09-30
Applicant: MITSUI PETROCHEMICAL IND
Inventor： TANAKA MICHIO , ISHIBASHI MASAYASU , TANIGUCHI KATSUO
Abstract: PURPOSE:To obtain the titled compound useful as a raw material for condensed polymer, etc., in high purity at a low cost, by using 3,3',5,5'-tetra-t-butyl-4,4'- dihydroxybiphenyl as a raw material and subjecting to dealkylation reaction under specific catalyst, solvent and temperature conditions. CONSTITUTION:The objective compound is produced by dealkylating 3,3',5,5'- tetra-t-butyl-4,4'-dihydroxybiphenyl at 150-300 deg.C, preferably 170-280 deg.C in the presence of an acid catalyst (e.g. sulfuric acid or sulfonic acid) using a solvent selected from a saturated hydrocarbon having a boiling point of >=190 deg.C, an alicyclic hydrocarbon having a boiling point of >=190 deg.C, a hydrocarbon having an iodine value of
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