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    PRODUCTION OF BIS(3-NITROPHENOXY) COMPOUND
    131.
    发明专利
    PRODUCTION OF BIS(3-NITROPHENOXY) COMPOUND 失效

    公开(公告)号：JPH03232842A

    公开(公告)日：1991-10-16

    申请号：JP30613890

    申请日：1990-11-14

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KASE MOTOHIRO ,  NAKAYAMA HITOSHI ,  WADA MASARU ,  NAGATA TERUYUKI ,  YAMAGUCHI TERUHIRO

    IPC: C07C201/12 ,  C07C205/38 ,  C07C315/04 ,  C07C317/22 ,  C07C319/20 ,  C07C323/20

    Abstract: PURPOSE:To obtain the subject compound on an industrial scale at a low cost by reacting a 4,4'-bisphenol compound with m-dinitrobenzene in a polar aprotic solvent in the presence of a base comprising particles of alkali metal carbonate and bicarbonate having diameter smaller than a specific level while removing water produced as a by-product. CONSTITUTION:A 4,4'-bisphenol compound of formula I [X is 1-20C bivalent hydrocarbon group, C(CF3)2, CO, S, SO, SO2, O or direct bond to bond the phenylene groups] is condensed with m-dinitrobenzene in the presence of a base to obtain bis(3-nitrophenoxy) compound of formula III. The condensation reaction is carried out by using a base comprising particles of an alkali metal carbonate and an alkali metal bicarbonate having particle diameter of

    PRODUCTION OF 3,4'-DIHYDROXYBIPHENYL
    133.
    发明专利
    PRODUCTION OF 3,4'-DIHYDROXYBIPHENYL 失效

    公开(公告)号：JPH01160931A

    公开(公告)日：1989-06-23

    申请号：JP31870387

    申请日：1987-12-18

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： MIURA TORU ,  WADA MASARU ,  FURUYA MASAYUKI ,  NAGATA TERUYUKI

    IPC: C07C37/06 ,  B01J27/232 ,  C07B61/00 ,  C07C27/00 ,  C07C37/50 ,  C07C39/15 ,  C07C67/00

    Abstract: PURPOSE:To obtain the title compound useful as a resin raw material for polyester, polyepoxide, etc., in industrial preparation, by subjecting 3,3-bis(4- hydroxyphenyl)-cyclohexanol which is a novel substance to decomposition and dehydrogenation reactions. CONSTITUTION:3,3-Bis (4-hydroxyphenyl)-cyclohexanol which is a novel substance obtained by reacting 3-hydroxycyclohexanone with phenol in the presence of catalysts is subjected to decomposition and dehydrogenation reactions at 100-400 deg.C, preferably 150-300 deg.C to obtain the 3,4'-dihydroxybiphenyl whose industrial preparation has not been entirely proposed in industrial preparation. Furthermore though in the abovementioned reactions, decomposition reaction and hydrogenation reaction can be carried out in separate processes, they are effective to carry out in one process and a base or acid catalyst is used in the decomposition reaction and well-known dehydrogenation catalyst is used in dehydrogenation reaction.

    PRODUCTION OF 2-(4-HYDROXYPHENYL)-CYCLOHEXANONE
    134.
    发明专利
    PRODUCTION OF 2-(4-HYDROXYPHENYL)-CYCLOHEXANONE 失效

    公开(公告)号：JPH01135739A

    公开(公告)日：1989-05-29

    申请号：JP29326887

    申请日：1987-11-20

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： MIURA TORU ,  WADA MASARU ,  FURUYA MASAYUKI ,  KIKUCHI NOBUSADA ,  NAGATA TERUYUKI

    IPC: C07C49/747 ,  C07C45/00 ,  C07C45/54 ,  C07C45/71 ,  C07C67/00

    Abstract: PURPOSE:To obtain the present compound which is a precursor of 2,4'-biphenol, useful as a monomer for polyesters, polycarbonates, etc., in high yield in a short process, by subjecting 2-hydroxycyclohexanone used as a raw material and phenol to condensation reaction. CONSTITUTION:2-Hydroxycyclohexanone or a dimer thereof as a raw material is condensed with phenol in the presence of preferably an acid catalyst and further a cocatalyst at 20-100 deg.C, preferably 30-70 deg.C to afford the aimed compound. The above-mentioned raw material is synthesized by a method for oxidizing 1,2-cyclohexanediol or hydrolyzing 2-cyclohexanone, etc. Since the aforementioned raw material compound is unstable and slowly converted into dimer even during preservation, the compound is normally marketed as the dimer, which can be used as the starting raw material. Furthermore, phenol is preferably used in an amount within the range of 2-10pts.wt. based on 100pts.wt. raw material.

    PRODUCTION OF HEXAHYDRO-2H-1,3-DIAZEPIN-2-ONS
    135.
    发明专利
    PRODUCTION OF HEXAHYDRO-2H-1,3-DIAZEPIN-2-ONS 失效

    公开(公告)号：JPS63107969A

    公开(公告)日：1988-05-12

    申请号：JP10439387

    申请日：1987-04-30

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KAJIMOTO NOBUYUKI ,  NAGATA TERUYUKI ,  WADA MASARU

    IPC: C07D243/04

    Abstract: PURPOSE:To industrially obtain the titled compound useful as an intermediate of medicine and agricultural chemicals and an aprotic and non-polar solvent directly in one stage in simple treatment, high yield and low price, by reacting diamines with phosgene, substantially using water and dehydrochloric agent. CONSTITUTION:Diamines such as N,N'-dimethyl-1,4-butanediamine, etc., expressed by formula I [R is H or lower alkyl; R' is (lower alkyl-substituted) tetramethylene] or as necessary salt thereof is reacted with stoichiometric phosgene of 1.0-1.5 times mole based on the diamines expressed by formula I in a water solvent while maintaining pH of 3.0-10.0, preferably 5.0-8.0 by dehydrochloride agent such as tert. amine, e.g. triethylamine preferably at 0-70 deg.C to provide the aimed compound expressed by formula II, used as a excellent aprotic and non-polar solvent for a polymer compound such as polyamides, polyvinylchloride, polystyrene, phenol resin, etc.

    PRODUCTION OF 2-IMIDAZOLIDINONE
    136.
    发明专利
    PRODUCTION OF 2-IMIDAZOLIDINONE 失效

    公开(公告)号：JPS62265268A

    公开(公告)日：1987-11-18

    申请号：JP10777086

    申请日：1986-05-13

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KAJIMOTO NOBUYUKI ,  NAGATA TERUYUKI ,  WADA MASARU

    IPC: C07D233/34

    Abstract: PURPOSE:To obtain the objective compound useful as an intermediate for pharmaceuticals and agricultural chemicals, with a simple operation in high yield at a low cost, by reacting 1,2-ethanediamine with phosgene in the presence of water and a dehydrochlorination agent in the reaction system. CONSTITUTION:2-Imidazolidinone useful also as an aprotic polar solvent can be produced by reacting 1,2-ethanediamine with phosgene in homogeneous state in the presence of water and a dehydrochlorination agent in the reaction system. The pH control during the reaction can be facilitated and the by-product hydrochloric acid can be scavenged in high efficiency to effect remarkable improvement of the yield of the objective compound. The pH of the reaction system is maintained at 3.0-10.0, especially 5.0-8.0 with the dehydrochlorination agent to suppress the by-production of 1,2-ethanediamine dicarbamine chloride, etc., resulting in further remarkable improvement of the yield of the objective compound. 1,2-Ethanediamine hydrochloride may be used as the raw material for the above reaction.

    COLOR DEVELOPING SHEET FOR PRESSURE-SENSITIVE COPY PAPER
    137.
    发明专利
    COLOR DEVELOPING SHEET FOR PRESSURE-SENSITIVE COPY PAPER 失效

    公开(公告)号：JPS62176875A

    公开(公告)日：1987-08-03

    申请号：JP1802786

    申请日：1986-01-31

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： YAMAGUCHI TERUHIRO ,  YAMAGUCHI KEISABURO ,  TANABE YOSHIMITSU ,  ASANO MAKOTO ,  WADA MASARU

    IPC: B41M5/155 ,  C08G61/02 ,  C08G61/10 ,  B41M5/12

    Abstract: PURPOSE:To obtain a color developing sheet for pressure-sensitive copy paper generating no yellowing due to light and gas such as nitrogen oxide in air, imparting a color image stable against light and a plasticizer and generating no lowering in developed color density and having good water resistance, by having a metallized substance of a copolycondensation resin consisting of salicylic acid and alpha,alpha'-dialkoxy-p-xylene contained as a developer. CONSTITUTION:A copolycondensation resin consisting of salicylic acid and alpha,alpha'-dialkoxy-p-xylene is obtained by reacting salicylic acid with alpha,alpha'-dialkoxy-p- xylene at 110 deg.C or more in the presence of an acid catalyst without almost generating corresponding side-reaction such as esterification reaction. A metallized substance of this salicylic acid copolycondensation resin is prepared by reacting an alkali metal salt of this resin and a water-soluble multivalent metal salt in water or in a solvent capable of dissolving both components. As the metal of the metallized substance, zinc is especially effective. As a method for preparing a color developing sheet for pressure-sensitive copy paper, there is the developer coating method or a method for internally adding the coupler in a paper stock during a papermaking process.

    PRODUCTION OF 1,3-DIMETHYL-2-IMIDAZOLIDINONE
    139.
    发明专利
    PRODUCTION OF 1,3-DIMETHYL-2-IMIDAZOLIDINONE 失效

    公开(公告)号：JPS61172862A

    公开(公告)日：1986-08-04

    申请号：JP1346285

    申请日：1985-01-29

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： NAGATA TERUYUKI ,  KAJIMOTO NOBUYUKI ,  WADA MASARU ,  NAKAYAMA HITOSHI ,  YAMADA TADAO

    IPC: C07D233/34 ,  C07D233/32

    Abstract: PURPOSE:To produce the titled substance useful as a polar aprotic solvent, in high yield, by reacting phosgene with N,N'-dimethylethylenediamine in the presence of water, while controlling the pH of the reaction system within a specific range with a dehydrochlorination agent. CONSTITUTION:The objective compound can be produced by reacting N,N'- dimethylethylenediamine and/or its hydrochloride with phosgene in the presence of water while controlling the pH of the reaction system to 3.0-10.0, preferably 4.0-9.0, especially 5.0-8.0 with a dehydrohalogenation agent. The dehydrohalogenation agent is preferably trimethylamine, dimethylaniline, pyridine, sodium hydroxide, etc., and its amount is 1.1-1.5 times the stoichiometric amount based on the diamine used as a raw material, and is nearly stoichiometric based on phosgene. The amount of water is preferably 5-30pts. wt. per 1pt. of the diamine used as a raw material.

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