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1. 发明授权

US4269768A Process for the preparation of chlorozincate salts of thiazolium azo dyestuffs 失效
标题翻译：制备噻唑鎓偶氮染料的氯酸锌盐的方法
公开(公告)号：US4269768A
公开(公告)日：1981-05-26
申请号：US54993
申请日：1979-07-06
申请人： Rudolf Neeb , Kurt Hohmann , Reinhard Mohr
发明人： Rudolf Neeb , Kurt Hohmann , Reinhard Mohr
IPC分类号： C09B29/00 , C09B29/08 , C09B44/00 , C09B44/20 , C09B45/00
CPC分类号： C09B44/005 , C09B29/0085 , C09B29/0807 , C09B44/20
摘要： 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.
摘要翻译：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

US4423226A Zinc chloride complex compounds 失效
公开(公告)号：US4423226A
公开(公告)日：1983-12-27
申请号：US243876
申请日：1981-03-16
申请人： Reinhard Mohr , Rudolf Neeb
发明人： Reinhard Mohr , Rudolf Neeb
IPC分类号： C07F3/06 , C07D209/88 , C07D265/38 , C09B19/00 , C07D209/82
CPC分类号： C07D265/38 , C07D209/88 , C09B19/00
摘要： 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

US4638053A 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 失效
标题翻译：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
公开(公告)号：US4638053A
公开(公告)日：1987-01-20
申请号：US775111
申请日：1985-09-11
申请人： Rudolf Neeb , Reinhard Mohr
发明人： Rudolf Neeb , Reinhard Mohr
IPC分类号： C09B44/00 , C09B44/20 , C09B69/06 , C09B29/045 , C09B43/11
CPC分类号： C09B44/005 , C09B44/20 , C09B69/065
摘要： 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.
摘要翻译：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。

4. 发明授权

US5756757A Process for the preparation of 3-hydroxy-N-benzimidazolon-5-yl-2-naphthamide in the high purity required of azo pigments 失效
标题翻译：制备高纯度3-偶氮颜料的3-羟基-N-苯并咪唑-5-基-2-萘甲酰胺的方法
公开(公告)号：US5756757A
公开(公告)日：1998-05-26
申请号：US559551
申请日：1995-11-16
申请人： Michael Meier , Heinrich Volk , Rudolf Neeb
发明人： Michael Meier , Heinrich Volk , Rudolf Neeb
IPC分类号： C07D235/26 , C09B29/20
CPC分类号： C07D235/26
摘要： The invention relates to a process for the preparation of 3-hydroxy-N-benzimidazolon-5-yl-2-naphthamide, which comprises reacting 5-aminobenzimidazolone and sodium carbonate in N-methylpyrrolidone with a solution of 3-hydroxy-2-naphthoyl chloride in xylene or toluene, filtering, washing with xylene or toluene, introducing the filter cake into water to which sodium carbonate has been added and steam-distilling, filtering off the residue with suction, washing and drying.
摘要翻译：本发明涉及一种制备3-羟基-N-苯并咪唑-5-基-2-萘甲酰胺的方法，该方法包括使5-氨基苯并咪唑酮与碳酸钠在N-甲基吡咯烷酮中的溶液与3-羟基-2-萘甲酰基氯化物在二甲苯或甲苯中，过滤，用二甲苯或甲苯洗涤，将滤饼引入加入碳酸钠的水中，蒸汽蒸馏，抽吸滤出残留物，洗涤和干燥。

5. 发明授权

US4916257A Process for the purification of 2-hydroxynaphthalene-6-carboxylic acid 失效
标题翻译：纯化2-羟基萘-6-羧酸的方法
公开(公告)号：US4916257A
公开(公告)日：1990-04-10
申请号：US296441
申请日：1989-01-12
申请人： Helmold von Plessen , Siegbert Rittner , Heinrich Volk , Werner Wykypiel , Rudolf Neeb
发明人： Helmold von Plessen , Siegbert Rittner , Heinrich Volk , Werner Wykypiel , Rudolf Neeb
IPC分类号： C07C51/00 , C07C51/43 , C07C65/11 , C07C67/00
CPC分类号： C07C51/43
摘要： The invention relates to a process for purification of 2-hydroxynaphthalene-6-carboxylic acid by recrystallization. In this process, the crude acid is recrystallized from water-miscible linear or cyclic aliphatic ethers, aliphatic polyethers or aliphatic hydroxy ethers or from at least 10% strength by weight aqueous solutions of these ethers. Recrystallization from a 35-90% strength by weight aqueous solutions of 1,4-dioxane is particularly preferred.
摘要翻译：本发明涉及通过重结晶纯化2-羟基萘-6-羧酸的方法。在该方法中，将粗酸从水混溶的线性或环状脂族醚，脂族聚醚或脂族羟基醚或这些醚的至少10重量％的重量水溶液中重结晶。特别优选从35-90％重量的1,4-二恶烷水溶液重结晶。

6. 发明授权

US4831168A Process for preparing 2-hydroxydibenzofuran-3-carboxylic acid and alkali metal salts thereof 失效
标题翻译：制备2-羟基二苯并呋喃-3-羧酸及其碱金属盐的方法
公开(公告)号：US4831168A
公开(公告)日：1989-05-16
申请号：US142333
申请日：1987-12-29
申请人： Rudolf Neeb , Wolfgang Ironich
发明人： Rudolf Neeb , Wolfgang Ironich
IPC分类号： C07D307/91
CPC分类号： C07D307/91
摘要： 2-Hydroxydibenzofuran-3-carboxylic acid and its alkali metal salts are prepared by reacting an alkali metal salt of 2-hydroxydibenzofuran with carbon dioxide, where appropriate under pressure, at a temperature above 120.degree. C. in an aliphatic alcohol of 4 to 8 carbon atoms.
摘要翻译： 2-羟基二苯并呋喃-3-羧酸及其碱金属盐的制备方法是，将2-羟基二苯并呋喃的碱金属盐与适当的压力下的二氧化碳在温度高于120℃的4至8的脂族醇中反应碳原子。

7. 发明授权

US4618701A Process for preparing 6-acetoxy-2-naphthoic-acid and pure 6-hydroxy-2-naphthoic acid 失效
标题翻译：制备6-乙酰氧基-2-萘甲酸和纯6-羟基-2-萘甲酸的方法
公开(公告)号：US4618701A
公开(公告)日：1986-10-21
申请号：US705626
申请日：1985-02-26
申请人： Rudolf Neeb , Wolfgang Ironich , Heinrich Volk
发明人： Rudolf Neeb , Wolfgang Ironich , Heinrich Volk
IPC分类号： C07C65/11 , C07C51/00 , C07C51/09 , C07C51/15 , C07C51/43 , C07C67/00 , C07C67/08 , C07C67/52 , C07C69/157 , C07C69/145
CPC分类号： C07C51/09 , C07C51/15
摘要： 6-Hydroxy-2-naphthoic acid can be selectively acetylated to 6-acetoxy-2-naphthoic acid, in particular in the presence of admixtures of isomeric hydroxy-naphthoic acids, and thus be separated from those isomeric admixtures. The acetylation is affected in aqueous alkaline solution by reaction with acetic anhydride. By hydrolysis of the 6-acetoxy-2-naphthoic acid, a pure 6-hydroxy-2-naphthoic acid is obtained.
摘要翻译： 6-羟基-2-萘甲酸可以选择性地乙酰化成6-乙酰氧基-2-萘甲酸，特别是在异构羟基 - 萘甲酸的混合物存在下，从而与这些异构体混合物分离。通过与乙酸酐反应，碱性水溶液中的乙酰化受影响。通过6-乙酰氧基-2-萘甲酸的水解，得到纯的6-羟基-2-萘甲酸。

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