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1. 发明专利

JPH09286862A PRODUCTION OF FLUOROSILICONE COMPOUND 失效
公开(公告)号：JPH09286862A
公开(公告)日：1997-11-04
申请号：JP10160996
申请日：1996-04-23
申请人： ASAHI GLASS CO LTD
发明人： FURUKAWA YUTAKA , KODERA MASAMI , KUMAI SEISAKU , JIERARUDO JIEI MAAFUII
IPC分类号： C08G77/22 , C08G77/385
摘要： PROBLEM TO BE SOLVED: To obtain a fluorosilicone compound being nonproblematic in the volatilization of the residual solvent even when used under high-temperature conditions by performing the reaction in the absence of a solvent in hydrosilylating a specified unsaturated fluoro computed with a hydrosilicone compound in the presence of a catalyst. SOLUTION: This compound is produced by performing the hydrosilylation in the substantial absence of a solvent in hydrosilyating an unsaturated fluoro compound represented by formula I (wherein R is a monovalent organic fluoro group; Q is a single bond or a divalent organic group; and R to R , which are independent of each other, are hydrogen atoms or monovalent organic groups) which a hydrosilicone compound having at least one Si-bonded hydrogen atom in the presence of a catalyst. In formula I, Q is desirably a single bond. All of R to R are more desirably hydrogen atoms. The monovalent organic fluoro group is particularly desirably a linear perfluoroalkyl represented by the formula: CF3 (CF2 )k (wherein (k) is an integer of 1-18).

2. 发明专利

JPH09268146A PRODUCTION OF OPTICALLY ACTIVE FLUORINE-CONTAINING HYDROXY COMPOUND 失效
公开(公告)号：JPH09268146A
公开(公告)日：1997-10-14
申请号：JP7904696
申请日：1996-04-01
申请人： ASAHI GLASS CO LTD
发明人： FUJIMA TOSHIHIKO , ASAI TOMOYUKI , KUMAI SEISAKU
IPC分类号： B01J25/02 , C07B61/00 , C07C29/145 , C07C31/38 , C07C67/28 , C07C69/24
摘要： PROBLEM TO BE SOLVED: To simply and efficiently obtain an optically active fluorine containing hydroxy compound which is useful as an intermediate for medicines and the like in high yield of asymmetric reduction by hydrogenating a readily available fluorine-containing ketone compound in the presence of a heterogeneous catalyst. SOLUTION: (A) A fluorine containing ketone compound of the formula; CHn F3-n -CO-R (n is 0, 1, 2; R is an alkyl, a haloalkyl, an acyl, an aralkyl, an aryl) is hydrogenated in the presence of (B) a nickel catalyst supporting an optically active compound to give (C) an optically active fluorine-containing hydroxy compound of the formula: CHn F3-n -CH*H(OH)-R. The component B preferably carries an optically active hydroxy acid or amino acid, particularly optically active tartaric acid. The amount of the optically active compound to be carried by the nickel; catalyst ids preferably 0.3-3 times the weight of the nickel component in the nickel catalyst.

3. 发明专利

JPH09241382A PRODUCTION OF FLUORINATED SILICONE COMPOUND 失效
公开(公告)号：JPH09241382A
公开(公告)日：1997-09-16
申请号：JP5347096
申请日：1996-03-11
申请人： ASAHI GLASS CO LTD
发明人： FURUKAWA YUTAKA , KODERA MASAMI , KUMAI SEISAKU
IPC分类号： C08G77/24 , C08G77/22 , C08G77/38 , C08G77/385
摘要： PROBLEM TO BE SOLVED: To prepare a silicone compound which does not gel even under high temperature conditions by reacting a terminally unsaturated compound with a compound obtained by the hydrosilylation of an unsaturated fluorinated compound. SOLUTION: An unsaturated fluorinated compound of formula I (where in R is a monovalent fluorinated organic group; Q is a single bond or a bivalent organic group; and R to R are each H or a monovalent organic group) is reacted with a hydrosilicone compound having at least two hydrogen atoms bonded to each silicon atom to obtain a reaction product containing a fluorinated hydrosilicone compound having an R -Q-CR R CR HCR R - group bonded to each silicon atom and a hydrogen atom bonded to each silicon atom. The reaction product is reacted with a terminally unsaturated compound of formula II(wherein R is H or a 1-6 C organic group) to obtain a fluorinated silicone compound which has an a R -Q-CR -R CR HCR R - group bonded to each silicon atom and a CH2 R CH2 group bonded to each silicon atom and is substantially free from hydrogen atoms bonded to silicon atoms.

4. 发明专利

JPH09235254A PRODUCTION OF 3-METHYL-6-NITRO-2,4,5-TRIHALOGENOBENZOIC ACID 失效
公开(公告)号：JPH09235254A
公开(公告)日：1997-09-09
申请号：JP4348796
申请日：1996-02-29
申请人： ASAHI GLASS CO LTD
发明人： SHIMIZU TAMAKI , ASAI TOMOYUKI , KUMAI SEISAKU
IPC分类号： C07C201/08 , C07C205/58
摘要： PROBLEM TO BE SOLVED: To obtain the subject compound in a good yield and in a short process, useful as an intermediate for a medicine or an agrochemical, especially as a synthetic intermediate for a fluoroquinoline-based antibacterial agent by using a reagent easy for handling. SOLUTION: This 3-methyl-6-nitro-2,4,5-trihalogenobenzoic acid of formula II is obtained by reacting a 3-methyl-2,4,5trihalogenobenzoic acid of formula I (X, Y are each a halogen) with a nitronium salt of the formula: NO2 Z (Z is a counter anion) at -70 to 100 deg.C. The nitronium salt is used by 1-100mol based on 1mol compound of the formula I, preferably 1-10mol, and 1-100 pts.wt. solvent based on 1 pts.wt. compound of formula I, preferably 2-30 pts.wt. is used.

5. 发明专利

JPH0967279A PRODUCTION OF UNSATURATED COMPOUND CONTAINING FLUORINE 失效
公开(公告)号：JPH0967279A
公开(公告)日：1997-03-11
申请号：JP22684495
申请日：1995-09-04
申请人： ASAHI GLASS CO LTD
发明人： OHARU KAZUYA , FUJIMA TOSHIHIKO , KUMAI SEISAKU
IPC分类号： C07C17/35 , C07C17/363 , C07C21/18 , C07C41/18 , C07C43/17
摘要： PROBLEM TO BE SOLVED: To provide a method for producing the subject compound effectively with a good productivity from easily available raw materials, not containing an impurity un-separable by a distillation and high in purity by reacting a hydroxy compound containing fluorine with a specific compound and then subjecting to a heat decomposition reaction. SOLUTION: This unsaturated compound containing fluorine of formula II is obtained by reacting a hydroxy compound containing fluorine of formula I (R' is a 1 20C univalent organic group containing fluorine; Q is a single bond or a bivalent organic group) with a compound selected from a carboxylic acid derivative of the formula R COX [R is H, a 1-4C alkyl ; X is a halogen, OR (R is H or a 1-4C alkyl), etc.] (suitably acetic acid, etc.), a phosphoric acid derivative of the formula (X ) (X ) (X )PO [X to X are each a halogen or OR (R is H or a 1-4C alkyl)] (e.g. phosphorus oxychloride), phosphorus pentoxide, metaphosphoric acid, pyrophosphoric acid or a polyphosphoric acid, and then sub jecting to a heat decomposition reaction. In reacting the compound of the formula I with the carboxylic acid derivative, the reaction is preferably performed at 50-150 deg.C under an atmospheric pressure for 0.1-10hr.

6. 发明专利

JPH0959215A PRODUCTION OF POLYFLUOROALKYL ESTER COMPOUND 失效
公开(公告)号：JPH0959215A
公开(公告)日：1997-03-04
申请号：JP20815795
申请日：1995-08-15
申请人： ASAHI GLASS CO LTD
发明人： FUJIMA TOSHIHIKO , OHARU KAZUYA , KUMAI SEISAKU
IPC分类号： C07C67/00 , C07C67/10 , C07C69/653
摘要： PROBLEM TO BE SOLVED: To easily obtain the subject compound useful as an intermediate for water-and-oil repellents, etc., in high yield under mild conditions, without the need of any hazardous reagent, by reaction of a specific polyfluoroalkylethane halide with a betaine compound followed by an alkali treatment. SOLUTION: This compound of the formula Rf -Q-(CH2 )2 OCOCR =CH2 is obtained by reaction between (A) a compound of the formula Rf -Q-(CH2 )2 X (Rf is a 1-20C polyfluoroalkyl; Q is a single bond or 1-4C alkylene; X is I or Br) and (B) a compound (hydrate) of the formula R R R N CH2 CHR COO (R is H or methyl; R is a 1-20C alkyl; R is a 1-5C alkyl) followed by an alkali treatment. The above reacting is pref. carried out in an alcohol solvent such as 1-butanol at 90-120 deg.C.

7. 发明专利

JPH08176307A PRODUCTION OF FLUOROSILICONE COMPOUND 失效
公开(公告)号：JPH08176307A
公开(公告)日：1996-07-09
申请号：JP25403295
申请日：1995-09-29
申请人： ASAHI GLASS CO LTD
发明人： FURUKAWA YUTAKA , KODERA MASAMI , KUMAI SEISAKU
IPC分类号： C07F7/18 , C08G77/38 , C08G77/385 , C08L83/07
摘要： PURPOSE: To easily obtain a useful fluorosilicone compound in industrially high yield without the need of using any special or expensive reagent, by reaction between a specific unsaturated fluorocompound and a hydrosilicone compound. CONSTITUTION: A compound of formula R -Q-X is first reacted with a compound of formula I to synthesize a compound of formula II, from which X and Y are eliminated into an unsaturated fluorocompound of formula III (R is a monovalent fluoroorganic group; Q is a single bond or divalent organic group; R to R are each H or a monovalent organic group; X is iodine, bromine or chlorine; Y is a monovalent group to be eliminated), which is then reacted with a hydrosilicone compound having at least one hydrogen atom bound to silicon atom to obtain the objective fluorosilicone compound having a group of formula IV bound to silicon atom. For the 1st reaction, azobisisobutyronitrile is used as a free radical initiator, and the elimination reaction is carried out in the presence of metallic zinc.

8. 发明专利

JPH08176032A PRODUCTION OF UNSATURATED COMPOUND CONTAINING FLUORINE 失效
公开(公告)号：JPH08176032A
公开(公告)日：1996-07-09
申请号：JP1440495
申请日：1995-01-31
申请人： ASAHI GLASS CO LTD
发明人： FURUKAWA YUTAKA , KODERA MASAMI , KUMAI SEISAKU
IPC分类号： C07B37/04 , C07C17/35 , C07C21/18 , C07C31/34 , C07C67/293 , C07C69/63 , C08F14/18
摘要： PURPOSE: To efficiently obtain the subject compound, useful as a raw material for industrial materials having excellent water and oil repellencies, mold releasability, etc., and capable of especially readily providing a silicone compound containing fluorine according to a specific method. CONSTITUTION: A compound of the formula Rf -Q-X (Rf is a monovalent organic group containing fluorine; Q is a single bond or a bivalent organic group; X is Cl, Br or Cl) is reacted with a compound of formula I (R to R are each H or a monovalent organic group), preferably in the presence of azobisisobutyronitrile which is a radical initiator to afford a compound of formula II. XY are then eliminated from the resultant compound of formula II by heating in the presence of zinc in an amount of 1.1-1.5mol based on 1mol compound. Thereby, the objective compound of formula III is obtained. Furthermore, the compound of formula I is preferably used in an amount of 1-1.5mol based on 1mol compound of the formula Rf -Q-X.

9. 发明专利

JPH0812604A TRIFLUORO-2-(TRANS-4-SUBSTITUTED CYCLOHEXYL)ETHYLENE AND ITS PRODUCTION 失效
公开(公告)号：JPH0812604A
公开(公告)日：1996-01-16
申请号：JP14348094
申请日：1994-06-24
申请人： ASAHI GLASS CO LTD
发明人： YOKOKOJI OSAMU , SHIMIZU TAMAKI , KUMAI SEISAKU
IPC分类号： C07D239/26 , C07C17/04 , C07C17/25 , C07C17/26 , C07C22/00 , C07C22/02 , C07C22/08 , C07C23/10 , C07C25/18 , C07C25/24 , C07C41/24 , C07C43/176 , C07C43/192 , C07C43/225 , C07C45/30 , C07C45/65 , C07C49/567 , C07C49/813 , C07C253/30 , C07C255/46 , C07C255/50 , C07D211/14 , C07D211/36 , C07D319/06 , C07D339/06 , C09K19/04 , C09K19/30 , C09K19/34
摘要： PURPOSE:To produce a new intermediate useful for synthesizing a liquid crystal compound, especially a liquid crystal compound useful for STN in a very high yield by very ready operations. CONSTITUTION:This compound is expressed by the formula [R is a 1 to 10C alkyl, a halogen or CN. in the case of an alkyl, 0 may be inserted in the alkyl or in the C-C bond between the alkyl and A or a part of C-C bonds may be replaced with triple bonds or double bonds. one CH2 in the alkyl may be replaced with CO or a part or the whole of H may be replaced with F; Cy is a non-substituted trans-1,4-cyclohexylene; A is trans-1,4-cyclohexyne, 1,4- phenylene or 1,4-cyclohexenylene which may be respectively substituted with a halogen or CN; (m) is 0 or 1], e.g. 2-(trans-4-n-propylcyclohexyl)-1,1,2-trifluoro- ethylene. This compound is synthesized by fluorinating a compound of formula II and conducting dehydrofluorination of the resultant compound of formula III.

10. 发明专利

JPH07165638A NEW FLUOROBENZOTRICHLORIDE COMPOUND 失效
公开(公告)号：JPH07165638A
公开(公告)日：1995-06-27
申请号：JP29652494
申请日：1994-11-30
申请人： ASAHI GLASS CO LTD , SEIMI CHEM KK
发明人： KUMAI SEISAKU , OHASHI MASAO , YAGINUMA YUTAKA , TAKEDA KATSUHIKO
IPC分类号： C07B61/00 , C07C25/13 , C07C51/093 , C07C63/70
摘要： PURPOSE:To obtain a new fluorobenzotrichloride compound useful as an intermediate for pharmaceuticals, etc., and safely and easily producible from a fluorobenzene compound on an industrial scale. CONSTITUTION:This new 4-fluorobenzotrichloride compound includes 2-chloro-4,5- difluorobenzotrichloride of formula III, 2,4,5-trifluorobenzotrichloride of formula IV, 2-bromo-4,5-difluorobenzotrichloride of formula V and 2,3,4-trichloro-5- fluorobenzotrichloride of formula VI. The compound of formula II (X1 and X3 each is F, Cl, Br or I; X2 is H, F, Cl, Br or I) collectively representing the compounds of formula III to formula VI can be produced by reacting a fluorobenzene of formula I in carbon tetrachloride in the presence of a Lewis acid catalyst. A fluorobenzoic acid can be produced in high purity and yield by the hydrolysis of the fluorobenzotrichloride compound of formula II.

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