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    PRODUCTION OF AZO COMPOUND
    1.
    发明专利
    PRODUCTION OF AZO COMPOUND 失效

    公开(公告)号：JPS61254550A

    公开(公告)日：1986-11-12

    申请号：JP9592985

    申请日：1985-05-08

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KAMICHI NOBUO ,  TAKAGUCHI TOMOAKI

    IPC: C09B41/00 ,  C07C67/00 ,  C07C301/00 ,  C07C303/32 ,  C07C309/50

    Abstract: PURPOSE:To obtain an azo compound useful as an intermediate for an acidic mordant dye or metal complex salt dye with a suppressed by-product without any problem in dyeing and fastness, by conducting coupling reaction of a diazo compound with beta-naphthol under nitrogon gas atmosphere. CONSTITUTION:Both diazo compound (example; 1-diazo-2-naphthol-4-sulfonic acid) expressed by formula I (X is H or nitro) and beta-naphthol are respectively dissolved in an aqueous solution of an alkali such as sodium hydroxide. Then after ammonium sulfate is added into the aqueous alkali solution of the diazo compound, the aqueous alkali solution of beta-naphthol is added thereto while blowing nitrogen gas thereinto, and the reaction solution is kept at 9.5-11.0PH and 30-70 deg.C to carry out the coupling reaction and obtain the aimed substance expressed by formula II. The reaction is carried out by using beta-naphthol in an amount of 1mol- a slight excess.

    SEPARATION OF 4*55DINITROCHRYSAZIN AND 4*88 DINITROANTHRARUFIN
    3.
    发明专利
    SEPARATION OF 4*55DINITROCHRYSAZIN AND 4*88 DINITROANTHRARUFIN 失效

    公开(公告)号：JPS55118443A

    公开(公告)日：1980-09-11

    申请号：JP2610179

    申请日：1979-03-08

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： FUJII SHIROU ,  AIGA HIROSHI ,  KAMICHI NOBUO

    IPC: C07C205/47 ,  C07C67/00 ,  C07C201/00

    Abstract: PURPOSE:To separate the title compounds useful as intermediates for bule disperse dye, mutually and readily, through the solubility difference in an aqueous alkali metal hydroxide. CONSTITUTION:4,5-Dinitrochrysazin and 4,8-dinitroanthrarufin or their alkali metal salts are separated mutually from their mixture through the solubility difference in an aqueous alkali metal hydroxide, without harmful mercury catalysts and separation of dinitroanthraquinone mixture in the method starting with the dinitration of anthraquinone. At first 4,5-dinitrochrysazin is dissolved in the aqueous solution as a salt at a lower concentration of the hydroxide, and then the salt is deposited at a higher concentration.

    SEPARATION OF MIXTURE OF 1*55 AND 1*88DINITROANTHRAQUINONE
    4.
    发明专利
    SEPARATION OF MIXTURE OF 1*55 AND 1*88DINITROANTHRAQUINONE 失效

    公开(公告)号：JPS55118442A

    公开(公告)日：1980-09-11

    申请号：JP2610079

    申请日：1979-03-08

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： FUJII SHIROU ,  AIGA HIROSHI ,  KAMICHI NOBUO

    IPC: C07C205/47 ,  C07C67/00 ,  C07C201/00

    Abstract: PURPOSE:To obtain the title isomers useful as starting materials for blue disperse dyes in high yield, readily and economically, by bringing crude dinitroanthraquinone mixture into contact with a small amount of a solvent, e.g. chlorobenzene. CONSTITUTION:1,5- and 1,8-Dinitroanthraquinone are separated, by bringing a dinitroanthraquinone mixture obtained through the dinitration of anthraquinone, most preferably in the mixing ratio of 1,5- to 1,8-isomers of 1:1, into contact with a solvent, e.g. mono- di-, or trichlorobenzene, solely or a mixture of two or more of these compounds, in an amount 2-10 times, preferably 3-8 times, that of the crude dinitroanthraquinone.

    SEPARATION OF 1*55DIPHENOXYANTHRAQUINONE AND 1*88 DIPHENOXYANTHRAQUINONE
    5.
    发明专利
    SEPARATION OF 1*55DIPHENOXYANTHRAQUINONE AND 1*88 DIPHENOXYANTHRAQUINONE 失效

    公开(公告)号：JPS55102535A

    公开(公告)日：1980-08-05

    申请号：JP876479

    申请日：1979-01-30

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： FUJII SHIROU ,  AIGA HIROSHI ,  KAMICHI NOBUO

    IPC: C07C50/34 ,  C07C45/00 ,  C07C46/10 ,  C07C67/00

    Abstract: PURPOSE:To prepare highly pure 1,5- and 1,8-diphenoxyanthraquinones useful as intermediates for production of dyes, separately, in high yield, by separating the mixture of 1,5- and 1,8-diphenoxyanthraquinones into the individual constituents, taking advantage of the difference of the solubilities and using a small amount of an inexpensive solvent in place of mercury. CONSTITUTION:An alcohol is added to the mixture of 1,5- and 1,8-diphenoxyanthraquinones obtained by the conventional phenoxylation. The alcohol is, e.g. methyl alcohol, ethyl alcohol, etc. The alcohol is slowly dropped into the mixture near the boiling point. The solution is cooled and filtered to give 1,5-diphenoxyanthraquinone having low solubility. 1,8-Diphenoxyanthraquinone having high solubility is deposited by cooling the filtrate or diluting it with an alchol and cooling the solution.

    PREPARATION OF 1-DIAZO-7-NITRO-2-NAPHTHOL-4-SULFONIC ACID
    7.
    发明专利
    PREPARATION OF 1-DIAZO-7-NITRO-2-NAPHTHOL-4-SULFONIC ACID 失效

    公开(公告)号：JPS61254551A

    公开(公告)日：1986-11-12

    申请号：JP9593085

    申请日：1985-05-08

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： KAMICHI NOBUO ,  TAKAGUCHI TOMOAKI

    IPC: C07C309/50 ,  C07C67/00 ,  C07C301/00 ,  C07C303/22

    Abstract: PURPOSE:To obtain a compound useful as a raw material for an acidic mordant dye or metal complex salt dye in high purity, by nitrating 1-diazo-2-naphthol-4- sulfonic acid, and treating the resultant product with a saline solution. CONSTITUTION:1-Diazo-2-naphthol-4-sulfonic acid is dissolved in a conc. sulfuric acid or a mixture of conc. sulfuric acid with fuming sulfuric acid, and nitrated at 5-9 deg.C by dropping mixed acid thereinto. The product is isolated by precipitating at

    PRODUCTION OF QUINOPHTHALONE DYE
    9.
    发明专利
    PRODUCTION OF QUINOPHTHALONE DYE 失效

    公开(公告)号：JPS55108460A

    公开(公告)日：1980-08-20

    申请号：JP1434279

    申请日：1979-02-13

    Applicant: MITSUI TOATSU CHEMICALS

    Inventor： AIGA HIROSHI ,  KAMICHI NOBUO

    IPC: C09B25/00

    Abstract: PURPOSE:To produce quinophthalone dye of good quality in high yields which does not contain carboxylic acid material, by reacting hydroxy-quinophthalone-carboxylic acid cpd. with an alcohol in the presence of sulfonic acid or sulfuric acid. CONSTITUTION:A cpd. of formula I (wherein X is H, halogen atom; Y is H, halogen atom, alkyl, alkoxy; n is 1 or 2) is reacted with an alcohol of formula ROH (wherein R is alkyl, cycloalkyl, alkenyl) in the presence of a cpd. of formula D-SO3H (wherein D is aliph. or arom. residue) or sulfuric acid. Examples of the cpd. of formula I are 3'-hydroxy-quinophthalone-4-carboxylic acid, 5-chloro-3'- hydroxy-quinophthalone-4-carboxylic acid, etc. Examples of the cpd. of formula D-SO3H are p-toluenesulfonic acid, benzenesulfonic acid, etc.

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