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    • 1. 发明授权
    • Process for the preparation of chlorozincate salts of thiazolium azo
dyestuffs
    • 制备噻唑鎓偶氮染料的氯酸锌盐的方法
    • US4269768A
    • 1981-05-26
    • US54993
    • 1979-07-06
    • Rudolf NeebKurt HohmannReinhard Mohr
    • Rudolf NeebKurt HohmannReinhard Mohr
    • C09B29/00C09B29/08C09B44/00C09B44/20C09B45/00
    • C09B44/005C09B29/0085C09B29/0807C09B44/20
    • Chlorozincate salts of thiazolium azo compounds are prepared by reacting thiazolium azo compounds with an dialkylsulfate having from 1 to 4 carbon atoms in the alkyl radicals, which process comprises carrying out the reaction in an aqueous medium at a temperature of from about 10.degree. to 50.degree. C. in the presence of a zinc compound capable of binding acid, and with the use of from 1.8 to 2.5 mols of the dialkylsulfate, calculated on the starting azo dyestuff, at a pH not exceeding 8, preferably at 3-7. The prepared thiazolium azo compound is precipitated as chlorozincate salt, especially by means of an alkali metal chloride. According to this process, the chlorozincate salts are obtained in higher purity. A perceptible decomposition of the thiazolium azo compound does not occur. Chemicals, for example the alkylation agent and acid-binding agents need be used in a small quantity. In addition to this economy and to the less pollution of the waste water, the process has the advantage that it can be carried out with the use of a small reaction volume.
    • 噻唑鎓偶氮化合物的氯化锌盐通过使噻唑鎓偶氮化合物与烷基中具有1至4个碳原子的二烷基硫酸盐反应制备,该方法包括在水介质中在约10°至50℃的温度下进行反应 在能够结合酸的锌化合物的存在下,并且使用1.8-2.5摩尔在起始偶氮染料上计算的二烷基硫酸盐,pH不超过8,优选3-7。 制备的噻唑鎓偶氮化合物作为氯酸锌盐,特别是通过碱金属氯化物沉淀。 根据该方法,得到较高纯度的氯锌酸盐。 不会发生噻唑鎓偶氮化合物的可察觉的分解。 化学品,例如烷基化剂和酸结合剂需要少量使用。 除了这种经济之外,对废水的污染较少,该方法的优点是可以使用小的反应体积进行。
    • 2. 发明授权
    • Zinc chloride complex compounds
    • US4423226A
    • 1983-12-27
    • US243876
    • 1981-03-16
    • Reinhard MohrRudolf Neeb
    • Reinhard MohrRudolf Neeb
    • C07F3/06C07D209/88C07D265/38C09B19/00C07D209/82
    • C07D265/38C07D209/88C09B19/00
    • Zinc chloride complex compounds to which the structure of the general formula (1) ##STR1## can be assigned, in which the individual radicals in the formula have the following meanings: Rhu 1 is a hydrogen atom or an optionally substituted lower alkyl group; R.sup.2 is a hydrogen atom, an optionally substituted lower alkyl group or an optionally substituted phenyl radical; R.sup.3 is a hydrogen atom or an optionally substituted lower alkyl group; R.sup.4 is a hydrogen atom, an optionally substituted lower alkyl group or an optionally substituted phenyl radical; R.sup.5 is a hydrogen atom or a halogen atom or a lower alkyl group or a lower alkoxy group, or R.sup.1 and R.sup.5 together form the o-phenylene radical; R.sup.6 is a hydrogen atom or a halogen atom or a lower alkyl group or a lower alkoxy group; Z is a hydrogen atom or a halogen atom or a lower alkyl group or a cyano, carboxylic acid, carbamoyl or sulfamoyl group or a carbamoyl or sulfamoyl group which is monosubstituted or disubstituted by lower alkyl, or a trifluoromethyl or lower carbalkoxy group, a lower alkoxy group which can be substituted by cyano, an acyloxy group, an acylamino group, a lower alkylamino group or a lower dialkylamino group. They are prepared by reacting a nitroso compound of the formula (2) ##STR2## in which R.sup.3, R.sup.4, R.sup.6 and Z have the meanings mentioned above, with an m-aminophenol of the formula (3) ##STR3## in which R.sup.1, R.sup.2 and R.sup.5 have the meanings mentioned above, in the presence of zinc chloride and in the absence of a base. The zinc chloride complex compounds of the formula (1) can be converted by eliminating the radical Z in the formula or by removing, by oxidative means, this radical Z, in the formula, which is in the ortho-position in relation to the nitrogen atom, or the other hydrogen atom which is in the ortho-position, into the phenoxazine dyestuffs of the formula (4) ##STR4## in which R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5 and R.sup.6 have the meanings mentioned above and Z.sub.1 denotes a halogen atom, a lower alkyl group, a cyano, carboxylic acid, carbamoyl or sulfamoyl group, a carbamoyl or sulfamoyl group which is monosubstituted or disubstituted by lower alkyl, or a trifluoromethyl or lower carbalkoxy group or a hydrogen atom and X.sup.(-) represents and anion.
    • 3. 发明授权
    • Process for the preparation of chlorozincate salts of benzo thiazolium
azo dyestuffs by alkylating with dialkylsulfate in aqueous medium in
the presence of Zn-containing acid acceptor at pH.ltoreq.7
    • 在含有Zn的酸受体的pH7中存在下,通过在含水介质中与二烷基硫酸盐烷基化制备苯并噻唑鎓偶氮染料的氯酸锌盐的方法
    • US4638053A
    • 1987-01-20
    • US775111
    • 1985-09-11
    • Rudolf NeebReinhard Mohr
    • Rudolf NeebReinhard Mohr
    • C09B44/00C09B44/20C09B69/06C09B29/045C09B43/11
    • C09B44/005C09B44/20C09B69/065
    • Chlorozincate salts of benzothiazonium azo compounds are prepared by reacting benzothiazolium azo compounds with an dialkylsulfate having from 1 to 4 carbon atoms in the alkyl radicals, which process comprises carrying out the reaction in an aqueous medium at a temperature of from 10.degree. to 80.degree. C. in the presence of an acid acceptor and the alkylation with the use of from 1.8 to 2.5 mols of the dialkylsulfate, calculated on the starting azo dyestuff, at a pH not exceeding 7. The prepared benzothiazolium azo compound is precipitated as chlorozincate salt, especially with the use of an alkali metal chloride. According to this process, the chlorozincate salts are obtained in higher purity. A perceptible decomposition of the benzothiazolium azo compound does not occur. Chemicals, for example the alkylation agent and acid-binding agents need be used in a small quantity. In addition to this economy and to the less pollution of the waste water, the process has the advantage that it can be carried out with the use of a small reaction volume.
    • 苯并噻唑偶氮化合物的氯化锌盐通过苯并噻唑鎓偶氮化合物与烷基中具有1至4个碳原子的二烷基硫酸盐反应来制备,该方法包括在水介质中在10至80℃的温度下进行反应 在酸性受体的存在下进行烷基化,并使用1.8-2.5摩尔在起始偶氮染料上计算的二烷基硫酸盐在pH不超过7的条件下进行烷基化。制备的苯并噻唑鎓偶氮化合物作为氯酸锌沉淀,特别是 使用碱金属氯化物。 根据该方法,得到较高纯度的氯锌酸盐。 不会发生苯并噻唑鎓偶氮化合物的可察觉的分解。 化学品,例如烷基化剂和酸结合剂需要少量使用。 除了这种经济之外,对废水的污染较少,该方法的优点是可以使用小的反应体积进行。