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1. 发明专利

JPH11116527A PRODUCTION OF 2-SUBSTITUTED-1,3-INDANEDIONE DERIVATIVE 失效
公开(公告)号：JPH11116527A
公开(公告)日：1999-04-27
申请号：JP27553497
申请日：1997-10-08
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , TANIGAWA YUICHI , HAMASHIMA KAORU
IPC分类号： C07C45/48 , C07C45/80 , C07C45/81 , C07C49/67 , C07C49/683 , C07C49/697 , C07C49/755
摘要： PROBLEM TO BE SOLVED: To provide a method for producing, in high yield, the subject compound useful as an intermediate for medicines and agrochemicals by adding water to a reaction mixture containing a specific indanedione derivative to separate it into the aqueous phase and organic solvent phase, and separating the water phase after keeping it at a specific pH level. SOLUTION: This compound is obtained by adding water to a reaction mixture containing a 2-substituted-1,3-indanedione derivative shown by formula III to transfer the derivative into the aqueous phase, separating the mixture into the aqueous phase and organic solvent phase, and separating the aqueous phase after keeping it at pH 4 to 8, wherein the compound shown by formula III is obtained by reacting an ester shown by formula I (R1 is a 1-10C alkyl, 2-10 alkenyl or the like; and R2 is a 1-4C alkyl) with a phthalic ester derivative shown by formula II (R3 is a 1-4 alkyl; R4 to R7 are each H, a 1-10C alkyl or the like) in the presence of a base (e.g. sodium hydride or sodium methoxide), preferably at 100 to 150 deg.C.

2. 发明专利

JP2000302773A PRODUCTION OF EPOXY COMPOUND 失效
公开(公告)号：JP2000302773A
公开(公告)日：2000-10-31
申请号：JP11177099
申请日：1999-04-20
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： C07D301/14 , C07D303/32
摘要： PROBLEM TO BE SOLVED: To obtain the subject epoxy compound that is useful as a herbicide with occurrence of an explosive atmosphere by purifying a compound bearing an ethylenically unsaturated double bond, then allowing the purified product to react with a peroxide. SOLUTION: A compound represented by formula I R is an indane-1,3-dione represented by formula II [R1 is H or a lower alkyl; B is a (substituted) benzene ring]; and A is a benzene ring which may be substituted with an H-free electron attracting group} is dissolved in an organic solvent (for example, peracetic acid in an amount of 2-10 times that of the compound of formula I) and fractionated with an aqueous solution in an amount of 1-5-fold that of the organic solvent at a pH of 2-5 at 40-80 deg.C to exclude a trace amount of metal that causes the autolysis of the peroxide.

3. 发明专利

JPH11158097A PRODUCTION OF ALCOHOLS 失效
公开(公告)号：JPH11158097A
公开(公告)日：1999-06-15
申请号：JP32569297
申请日：1997-11-27
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , KATOGI MAMORU , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： C07C29/40 , C07C33/30 , C07C33/48
摘要： PROBLEM TO BE SOLVED: To obtain the subject compound useful as an intermediate for medicines and agrochemicals, by reacting a specific organic halide with magnesium and paraformaldehyde and hydrolyzing the reaction product. SOLUTION: Magnesium and paraformaldehyde are suspended in a reaction solvent (e.g. diethyl ether; tetrahydrofuran or the like) at preferably 20-70 deg.C with stirring and is reacted with an organic halide of the formula RXn (R is an aromatic residue, an unsaturated aliphatic residue or the like; X is a halogen; (n) is >=1) preferably at 20-70 deg.C and then the reaction product is hydrolyzed at preferably 5-50 deg.C to give an alcohol of the formula R(CH2 OH)n . The organic halide is preferably a styrene derivative of the formula [A is a (substituted) benzene ring]. The amount of magnesium used is preferably 80-150 mol.% based on the organic halide.

4. 发明专利

JPH11343253A PRODUCTION OF ALPHA, BETA-DIBROMOETHYLBENZENE AND ALPHA-BROMOSTYRENE 失效
公开(公告)号：JPH11343253A
公开(公告)日：1999-12-14
申请号：JP14730298
申请日：1998-05-28
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： B01J27/08 , C07B61/00 , C07C17/14 , C07C17/25 , C07C22/04
摘要： PROBLEM TO BE SOLVED: To industrially advantageously obtain an α,β-dibromoethylbenzene useful as an intermediate for medicinals and agrochemicals by reacting a specific bromoethylbenzene with bromine in the presence of iodine so as to raise the reaction rate. SOLUTION: This compound, an α,β-dibromoethylbenzene of formula II (e.g. 3-chloro-α,β-dibromoethylbenzene), is obtained by reaction of (A) an α- bromoethylbenzene of formula I (A is a benzene ring optionally having H-free electron-attracting group (s)) with (B) bromine in the presence of iodine; wherein it is recommended that the amount of the component B to be used, for example, 0.5-3 molar times that of the component A, and the component B is dripped onto the component A at 0-200 deg.C for 30 min to 20 h or so followed by carrying out the reaction for 1-5 h.

5. 发明专利

JPH1192413A PRODUCTION OF 2-SUBSTITUTED-1,3-INDANEDIONE DERIVATIVE 失效
公开(公告)号：JPH1192413A
公开(公告)日：1999-04-06
申请号：JP25951197
申请日：1997-09-25
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , TANIGAWA YUICHI , HAMASHIMA KAORU
IPC分类号： B01J31/02 , C07B61/00 , C07C45/45 , C07C49/67
摘要： PROBLEM TO BE SOLVED: To obtain the subject derivative useful as an intermediate for medicines and agrochemicals in a high yield by reacting a specific phthalate ester derivative with a specified ester added by a specific feeding method in the presence of a base. SOLUTION: This method for producing a 2-substituted-1,3-indanedione derivative of formula II comprises reacting (A) 1 mole of a phthalate ester derivative of formula I (R3 is a 1-4C alkyl; R4-R7 are each H, a 1-10C alkyl, a 2-10C alkenyl or the like) with (B) 0.5-1.0 mole of an ester of the formula: R1CH2 COOR2 (R1 is a 1-10C alkyl, a 2-10C alkenyl, a 2-10C alkynyl; R2 is a 1-4C alkyl) in the presence of a base such as e.g. sodium hydride or sodium methoxide at 0-300 deg.C. Therein, the component B is dividedly added.

6. 发明专利

JPH09201539A METHOD FOR PURIFYING ION EXCHANGE RESIN 失效
公开(公告)号：JPH09201539A
公开(公告)日：1997-08-05
申请号：JP1372396
申请日：1996-01-30
申请人： MITSUBISHI CHEM CORP
发明人： SAKAGUCHI HIROTO , KATOGI MAMORU , TANIGAWA YUICHI , IKEDA YOSHIYA
IPC分类号： B01J47/00 , C08G65/02 , C08G65/30
摘要： PROBLEM TO BE SOLVED: To remove a trace of water soluble impurities in an ion exchange resin by a method in which the resin, after being swelled by washing with water, is contracted by being contacted with a water soluble organic solvent to discharge the impurities outside the resin. SOLUTION: An ion exchange resin is washed with water to remove impurities and to be swelled simultaneously. Next, the swelled resin is brought into contact with a water soluble organic solvent such as acetone and methanol to reduce its volume to two-thirds or less, discharging water soluble impurities left in the resin after the washing. In this way, the water soluble impurities left in the resin for oral drugs in particular can be removed efficiently.

7. 发明专利

JPH11228552A PRODUCTION OF EPOXY COMPOUND 失效
公开(公告)号：JPH11228552A
公开(公告)日：1999-08-24
申请号：JP3568598
申请日：1998-02-18
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： C07D301/14 , C07D303/32
摘要： PROBLEM TO BE SOLVED: To provide a method for producing an epoxy compound by dissolving a compound having an ethylenically unsaturated double bond in a solvent, filtering the solution through a filter and subsequently reacting the filtrate with a peroxide, capable of profitably obtaining the subject compound useful as an agrochemical, while largely inhibiting the decomposition of the peroxide to prevent the generation of explosion. SOLUTION: (A) A compound having an ethylenically unsaturated double bond for example, 2-[2-(3-chlorophenyl)-2-propenyl]-2-ethylindan-1,3-dione} is dissolved in (B) a solvent such as toluene, filtered through a filter made from Teflon (R) preferably having a filtration accuracy of 0.1-10 μm, and subsequently reacted with (C) a peroxide preferably at 50-100 deg.C to oxidize the unsaturated double bond, thus obtaining the objective compound 2-[2-(3- chlorophenyl)-2,3-epoxypropyl]-2-ethylindan-1,3-dione}. The component C is preferably an equilibrium peracetic acid prepared from hydrogen peroxide and acetic acid in the presence of an excessive amount of the acid.

8. 发明专利

JPH11171808A PRODUCTION OF ALPHA-BROMOSTYRENES 失效
公开(公告)号：JPH11171808A
公开(公告)日：1999-06-29
申请号：JP33852797
申请日：1997-12-09
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , HAMASHIMA KAORU , KAWAMURA SHIGENORI , TANIGAWA YUICHI
IPC分类号： B01J31/02 , C07B61/00 , C07C17/14 , C07C17/25 , C07C22/04
摘要： PROBLEM TO BE SOLVED: To provide a method for producing α-bromostyrenes by which the generation of by-products is prevented by extremely suppressing side reactions by removing bromine present in a system after bromination of α- bromoethylbenzene and before dehydrobromination reaction in one pot. SOLUTION: This method for producing the objective compound of formula III by reacting α-bromoethylbenzenes of formula I (A is benzene ring) with bromine and successively carrying out a dehydrobromination reaction of the obtained α,β-dibromoethylbenzene of formula II in the same reaction vessel comprises decreasing the remaining amount of the bromine in the system before the dehydrobromination reaction. The decrease of the bromine is preferably carried out by degrading the bromine by using a reluctant. The reluctant is preferably sodium hydrogen sulfite. The temperature for the treatment is preferably 10-30 deg.C. Preferably, the dehydrobromination reaction of the compound of formula I is carried out in the presence of a phase transfer catalyst in an aqueous medium by allowing a base to act on the compound, because the reaction proceeds in the aqueous medium and the aftertreatment becomes easier. The phase transfer catalyst is preferably a quarternary ammonium salts.

9. 发明专利

JPH11158095A PRODUCTION OF ALCOHOLS 失效
公开(公告)号：JPH11158095A
公开(公告)日：1999-06-15
申请号：JP32569397
申请日：1997-11-27
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , KATOGI MAMORU , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： C07C29/40 , C07B61/00 , C07C33/30 , C07C33/48
摘要： PROBLEM TO BE SOLVED: To obtain the subject compound having a high reaction rate, useful as an intermediate for medicines, agrochemicals, etc., by reacting a Grignard reagent with paraformaldehyde in the presence of an alkali and hydrolyzing the reaction product. SOLUTION: A Grignard reagent in an amount of 1 equivalent is reacted with preferably 0.8-1.5 equivalent of paraformaldehyde in the presence of preferably 0.005-0.1 pt.wt. based on the Grignard reagent of an organic amine (e.g. trimethylamine, pyridine or the like) by using preferably a solvent (e.g. diethyl ether, tetrahydrofuran or the like) of 1-15 times as much as the Grignard reagent at 20-70C for 30 minutes to 4 hours and then the reaction product is hydrolyzed to give an alcohol. The Grignard reagent is a compound of the formula RMgX (R is an aromatic residue, an unsaturated aliphatic residue or the like; X is a halogen; (n) is >=1), more preferably a compound of formula I [A is a (substituted) benzene ring)].

10. 发明专利

JP2002155048A METHOD FOR STABILIZING ORGANIC PERACID 失效
公开(公告)号：JP2002155048A
公开(公告)日：2002-05-28
申请号：JP2000355529
申请日：2000-11-22
申请人： MITSUBISHI CHEM CORP
发明人： HASHIMOTO HIDEYOSHI , HAMASHIMA KAORU , TANIGAWA YUICHI
IPC分类号： C07C409/26 , C07B63/04 , C07C409/24
摘要： PROBLEM TO BE SOLVED: To provide a stabilizer which can effectively inhibit the decomposition of an organic peracid, is inexpensive and is scarcely toxic, and to provide a method for stabilizing the organic peracid with the same. SOLUTION: 1. This method for stabilizing the organic peroxide, characterized by adding ethylenediaminetetraacetic acid compound and a phosphoric acid compound as stabilizers to an organic peroxide solution. 2. The stabilizer for the organic peracid, containing the ethylenediaminetetraacetic acid compound and the phosphoric acid compound.

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