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31. 发明授权

US4267346A Process for the preparation of 1,2,4-triazole 失效
标题翻译：制备1,2,4-三唑的方法
公开(公告)号：US4267346A
公开(公告)日：1981-05-12
申请号：US612
申请日：1979-01-02
申请人： Reinhard Kaiser , Guido Steffan
发明人： Reinhard Kaiser , Guido Steffan
IPC分类号： C07D249/08
CPC分类号： C07D249/08
摘要： A process for preparing 1,2,4-triazole which comprises contacting hydrazine with formamide in the molar ratio of 1:2.0-2.7 at a temperature from 100.degree. to 250.degree. C. in the presence of ammonia.
摘要翻译：一种制备1,2,4-三唑的方法，其包括在氨存在下，在100-250℃的温度下，使肼与甲酰胺以1:2.0-2.7的摩尔比接触。

32. 发明授权

US06369259B1 Method of preparing 4,5,6-trichloro-and 2,4,5,6-tetrachloropyrimidine 失效
标题翻译：制备4,5,6-三氯 - 和2,4,5,6-四氯嘧啶的方法
公开(公告)号：US06369259B1
公开(公告)日：2002-04-09
申请号：US09668087
申请日：2000-09-22
申请人： Guido Steffan , Georg Hardenbicker
发明人： Guido Steffan , Georg Hardenbicker
IPC分类号： C07C25503
CPC分类号： C07D239/30 , C07C255/24
摘要： Crystals with an average crystal size of ≦10 &mgr;m comprising compounds of the formula Ia and/or IIa A process for making said crystals.
摘要翻译：平均晶体尺寸<10μm的晶体包含用于制备所述晶体的式Ia和/或IIaA化合物的方法。

33. 发明授权

US06355827B1 Process for preparing 2-cyanoindan-1-ones 失效
标题翻译： 2-氰基茚满-1-酮的制备方法
公开(公告)号：US06355827B1
公开(公告)日：2002-03-12
申请号：US09485957
申请日：2000-02-18
申请人： Joachim Komoschinski , Helmut Fiege , Guido Steffan
发明人： Joachim Komoschinski , Helmut Fiege , Guido Steffan
IPC分类号： C07C25314
CPC分类号： C07C253/14 , C07C2602/08 , C07C255/47
摘要： In a particularly advantageous process for producing 2-cyanoindan-1-ones from 2-halogenated indan-1-ones by reaction with a cyanide salt, the cyanide salt is dissolved in a dipolar aprotic solvent or in a water-miscible ether and 2-halogenated indan-1-one is metered into this solution.
摘要翻译：在通过与氰化物盐反应从2-卤代茚满-1-酮生成2-氰基茚满-1-酮的特别有利的方法中，将氰化物盐溶于偶极非质子溶剂或水混溶性醚中，将卤代茚满-1-酮计量加入该溶液中。

34. 发明授权

US06197964B1 Method for the production of 2,6-dichloro-5-fluoronicotinonitrile and the chemical compound 3-cyano-2-hydroxy-5-fluoropyride-6-one-monosodium salt its tautomers 失效
标题翻译：制备2,6-二氯-5-氟烟腈的方法及其化合物3-氰基-2-羟基-5-氟吡啶-6-酮单钠盐其互变异构体
公开(公告)号：US06197964B1
公开(公告)日：2001-03-06
申请号：US09402047
申请日：1999-09-27
申请人： Andreas Sattler , Guido Steffan , Bernd Griehsel
发明人： Andreas Sattler , Guido Steffan , Bernd Griehsel
IPC分类号： C07D21384
CPC分类号： C07B39/00 , C07D213/85
摘要： The process according to the invention can be illustrated by way of example by the following equation: The monosodium salt of the 3-cyano-2-hydroxy-5-fluoropyrid-6-one (cf. Formula (I)) and/or tautomers thereof are preferably employed in the process according to the invention. The use of a basic catalyst enables significantly lower amounts of chlorinating agent to be employed in the chlorination according to the invention than is necessary, for example, for chlorination of the free dihydroxy compound according to EP-A 333 020. Furthermore, the product 2,6-dichloro-5-fluoronicotinonitrile is obtained in a high purity and high yields after hydrolysis, which is not the case if the conditions according to EP-A 333 020 are applied. Basic catalysts which can be used for the process according to the invention are, for example, organic bases, for example aliphatic and aromatic amines and amides, and also inorganic bases, for example basic compounds of nitrogen and phosphorus and salts thereof. Preferred basic catalysts are: pyridine, pyridines alkylated with 1 to 3 C1-C6-alkyl groups, piperidine, piperidines, imidazoles and indoles alkylated with 1 to 3 C1-C6-alkyl groups, N—C1-C6-alkylaminopyridines, N—di-C1-C6-alkylated anilines, tertiary N—C1-C6-alkylamines, urea and urea derivatives. Particularly preferred basic catalysts are triethylamine, urea and ethylpiperidine.
摘要翻译：根据本发明的方法可以通过以下方程式举例说明：3-氰基-2-羟基-5-氟吡啶-6-酮的单钠盐（参见式（I））和/或互变异构体优选使用根据本发明的方法。碱性催化剂的使用使得根据本发明的氯化中所使用的氯化剂的量显着更低，例如根据需要氯化游离二羟基化合物，至EP-A 333 020.此外，产生2,6-二氯-5-氟烟腈的方法是在水解后以高纯度和高产率获得的，如果应用根据EP-A 333 020的条件，则不是这种情况。可用于本发明方法的碱性催化剂是例如有机碱，例如脂族和芳族胺和酰胺，以及无机碱，例如氮和磷的碱性化合物及其盐。优选的碱性催化剂是：吡啶，用1至3个C 1 -C 6 - 烷基烷基化的吡啶，哌啶，哌啶，咪唑和用1至3个C 1 -C 6 - 烷基烷基化的吲哚，N-C 1 -C 6 - 烷基氨基吡啶，N-二 -C 1 -C 6烷基化苯胺，叔N-C 1 -C 6烷基胺，脲和脲衍生物。特别优选的碱性催化剂是三乙胺，尿素和乙基哌啶。

35. 发明授权

US5969152A Process for the preparation of nitropyrazole esters 失效
标题翻译：硝基吡唑酯的制备方法
公开(公告)号：US5969152A
公开(公告)日：1999-10-19
申请号：US888889
申请日：1997-07-07
申请人： Lutz Heuer , Nikolaus Muller , Guido Steffan
发明人： Lutz Heuer , Nikolaus Muller , Guido Steffan
IPC分类号： C07D231/10 , C07D231/16 , C07D231/14
CPC分类号： C07D231/16
摘要： Nitropyrazole esters of the formula ##STR1## in which R.sup.1 represents C.sub.1 -C.sub.6 -alkyl, are prepared by nitration of the corresponding pyrazole esters. The nitropyrazole esters permit the preparation of a known nitropyrazole amide in a particularly simple and economical manner and thereby improve the preparation of active compounds which are accessible from the nitropyrazole amide.
摘要翻译：通过硝化相应的吡唑酯制备其中R 1表示C 1 -C 6 - 烷基的式的硝基吡唑酯。硝基吡唑酯可以以特别简单和经济的方式制备已知的硝基吡唑酰胺，从而改进可从硝基吡唑酰胺获得的活性化合物的制备。

36. 发明授权

US5677453A Process for the preparation of 4,6-dichloropyrimidines 失效
标题翻译：制备4,6-二氯嘧啶的方法
公开(公告)号：US5677453A
公开(公告)日：1997-10-14
申请号：US699812
申请日：1996-08-19
申请人： Gunther Cramm , Volker Kass , Guido Steffan
发明人： Gunther Cramm , Volker Kass , Guido Steffan
IPC分类号： C07D239/30
CPC分类号： C07D239/30
摘要： 4,6-Dichloropyrimidines are obtained by the reaction of 4,6-dihydroxypyrimidines with excess phosphoryl chloride in a particularly advantageous manner when no base is added, during and/or after the reaction 0.75 to 1.5 mol of phosphorus trichloride and 0.7 to 1.3 mol of chlorine are added per equivalent of exchanged hydroxyl groups so that an excess of phosphorus trichloride with respect to chlorine is always present, and finally phosphorus trichloride and phosphoryl chloride are separated off. This process can be carried out in a particularly simple manner and also continuously.
摘要翻译：当没有碱被加入时，反应期间和/或之后，通过4,6-二羟基嘧啶与过量的磷酰氯的反应，得到4,6-二氯嘧啶，其中0.75-1.5摩尔三氯化磷和0.7-1.3摩尔每当量交换的羟基加入氯，以致总是存在相对于氯过量的三氯化磷，最后分离出三氯化磷和磷酰氯。该过程可以以特别简单的方式并且连续地进行。

37. 发明授权

US5144065A Process for the preparation of aminoarylsulphonic acids 失效
标题翻译：制备氨基磺酸的方法
公开(公告)号：US5144065A
公开(公告)日：1992-09-01
申请号：US737635
申请日：1991-07-30
申请人： Guido Steffan
发明人： Guido Steffan
IPC分类号： B01J25/00 , B01J10/00 , B01J19/26 , C07B61/00 , C07C303/22 , C07C309/46 , C07C309/47
CPC分类号： B01J10/002 , B01J19/26 , C07C303/22 , B01J2219/00083
摘要： In the process according to the invention for the preparation of aminoarylsulphonic acids by catalytic hydrogenation of nitroarylsulphonic acids, a substantial increase in the space-time yield in combination with reduced consumption of the catalyst is achieved by dispersing the hydrogen more finely and by limiting according to the invention the concentration of the nitroarylsulphonic acids to be hydrogenated.
摘要翻译：在根据本发明的用于通过硝基芳基磺酸的催化氢化制备氨基芳基磺酸的方法中，通过分散氢气更精细地分散氢气，并且通过根据本发明将待氢化的硝基芳基磺酸的浓度。

38. 发明授权

US4348334A Process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid (nitro-Armstrong's acid) 失效
标题翻译：制备3-硝基 - 萘-1,5-二磺酸镁盐（硝基 - 阿姆斯壮酸）的方法
公开(公告)号：US4348334A
公开(公告)日：1982-09-07
申请号：US113412
申请日：1980-01-18
申请人： Bernhard Albrecht , Hans Frey , Vinzenz Habermacher , Horst Behre , Lutz Kienitz , Wolfgang Schenk , Guido Steffan , Axel Vogel
发明人： Bernhard Albrecht , Hans Frey , Vinzenz Habermacher , Horst Behre , Lutz Kienitz , Wolfgang Schenk , Guido Steffan , Axel Vogel
IPC分类号： C07C309/40 , C07C67/00 , C07C301/00 , C07C303/06 , C07C303/22 , C07C303/32 , C07C143/55
CPC分类号： C07C309/00
摘要： A process for producing the magnesium salt of 3-nitro-naphthalene-1,5-disulfonic acid by sulfonating naphthalene, nitrating the sulfonation product, and separating the pure magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid, which process comprises:(a) sulfonating naphthalene with liquid SO.sub.3 in the presence of an inert organic solvent at temperatures between -40.degree. and +20.degree. C.;(b) adding to the reaction mixture obtained a mixture consisting of about equal parts of 100% sulfuric acid and fully reacted crude nitration mixture from nitration of a previous nitration charge, separating from the resulting two-phase system the upper organic solvent phase by decanting, and removing from the Armstrong's acid anhydride acid slurry the remainder of organic solvent by distillation, or removing it during or after subsequent nitration, subsequently adding to the residue the amount of nitric acid required for nitration, and then nitrating;(c) adding then firstly water and afterwards, in the absence of the inert organic solvent, at 90.degree. to 120.degree. C., a compound releasing magnesium ions, the amount being such that, per mol of 3-nitronaphthalene-1,5-disulfonic acid, 1.1 to 1.3 mols of magnesium ions are added, and a sulfuric acid concentration of between 40 and 60 percent by weight (relative to the sulfuric acid and water) is maintained; and(d) separating the crystallized magnesium salt of 3-nitronaphthalene-1,5-disulfonic acid at a temperature of between 20.degree. and 70.degree. C., and subsequently optionally washing it with a maximum of 60 percent by weight of sulfuric acid and/or water, and optionally drying the product.
摘要翻译：通过磺化萘，硝化磺化产物和分离3-硝基萘-1,5-二磺酸的纯镁盐来生产3-硝基 - 萘-1,5-二磺酸的镁盐的方法，该方法包括：（a）在-40℃〜+ 20℃的温度下，在惰性有机溶剂的存在下，用液态SO 3磺化萘。（b）向反应混合物中加入由约等量的100％硫酸组成的混合物和来自先前硝化装置的硝化的完全反应的粗硝化混合物，通过倾析从所得两相体系中分离出上部有机溶剂相，并通过蒸馏从阿姆斯壮的酸酐酸浆中除去剩余的有机溶剂，或者在后续硝化过程中或之后将其除去，随后向残余物中加入硝化所需的硝酸量，然后硝化; （c）然后首先加入水，然后在不存在惰性有机溶剂的情况下，在90〜120℃下，加入释放镁离子的化合物，其用量为每摩尔3-硝基萘-1,5 二磺酸，加入1.1〜1.3摩尔的镁离子，硫酸浓度保持在40〜60重量％之间（相对于硫酸和水）; 和（d）在20℃至70℃的温度下分离3-硝基萘-1,5-二磺酸的结晶镁盐，随后任选地用最多60重量％的硫酸洗涤， /或水，并任选地干燥产品。

39. 发明授权

US4341720A Process for the preparation of oxalyl chloride 失效
标题翻译：草酰氯的制备方法
公开(公告)号：US4341720A
公开(公告)日：1982-07-27
申请号：US247186
申请日：1981-03-24
申请人： Axel Vogel , Guido Steffan , Karl Mannes , Viktor Trescher
发明人： Axel Vogel , Guido Steffan , Karl Mannes , Viktor Trescher
IPC分类号： C07C55/36 , C07C51/00 , C07C51/60 , C07C67/00 , C07C57/00
CPC分类号： C07C51/60
摘要： In a process for the preparation of oxalyl chloride from an oxalic acid compound of the formula ##STR1## wherein R.sup.1 and R.sup.2 are identical or different and represent hydrogen or a lower alkyl radical,and phosphorus pentachloride in the presence of phosphorus oxychloride, the improvement wherein the reaction is carried out in the presence of an amino compound of the formula ##STR2## wherein R.sup.3 represents alkyl, aralkyl, aryl or an acyl group, optionally substituted by amino or carboxamido andR.sup.4 and R.sup.5 are identical or different and represent hydrogen or alkyl, aralkyl, or aryl, optionally substituted by amino or carboxamido, orR.sup.4 and R.sup.5 are linked in an optionally substituted carbocyclic ring with 5 to 7 ring members, which optionally contains nitrogen, sulphur and/or oxygen and is optionally substituted by alkyl, aralkyl, aryl and/or amino groups, andR.sup.3 represents hydrogen or alkyl, which can be linked with R.sup.4 to form a carbocyclic ring, aralkyl or aryl, optionally substituted by an amino or carboxamido group, or optionally forms a double bond in one of the radials R.sup.4 or R.sup.5,and the oxalyl chloride formed is distilled off during the reaction.
摘要翻译：在通式“IMAGE”的草酸化合物（其中R 1和R 2相同或不同并且代表氢或低级烷基）和五氯化磷在磷酰氯存在下制备草酰氯的方法中，该反应在下式的氨基化合物存在下进行：其中R 3表示烷基，芳烷基，芳基或酰基，任选被氨基或甲酰氨基取代，R 4和R 5相同或不同，表示氢或烷基，芳烷基或芳基，其任选被氨基或羧酰氨基取代，或R 4和R 5在任选取代的碳环中与5至7个环成员连接，所述环成员任选地含有氮，硫和/或氧并且任选地被烷基，芳烷基，芳基和/或氨基，并且R 3表示氢或烷基，其可以与R 4连接形成碳环，芳烷基或芳基，任选被上位体取代或者在一个径向R4或R5中任选形成双键，并且在反应期间蒸馏形成的草酰氯。

40. 发明授权

US4163752A Process for the preparation of aminonaphthalenesulphonic acids 失效
标题翻译：制备氨基萘磺酸的方法
公开(公告)号：US4163752A
公开(公告)日：1979-08-07
申请号：US868558
申请日：1978-01-11
申请人： Otto Barth , Hans-Joachim Becker , Horst Behre , Reinhard Kaiser , Guido Steffan , Jurgen Zander
发明人： Otto Barth , Hans-Joachim Becker , Horst Behre , Reinhard Kaiser , Guido Steffan , Jurgen Zander
IPC分类号： C07C309/47 , C07C67/00 , C07C301/00 , C07C303/22 , C07C303/32 , C07C143/56
摘要： A process has been invented for the preparation of aminonaphthalenesulphonic acids by the catalytic hydrogenation of salts of nitronaphthalenesulphonic acids with hydrogen in the presence of Raney nickel catalysts at elevated temperature and pressure, said catalysts comprising a combination of fresh Raney nickel catalyst and Raney nickel catalyst which has already been used in prior hydrogenation or hydrogenations.
摘要翻译：已经发明了一种通过在高温和高压下在阮内镍催化剂存在下通过硝基萘磺酸的盐催化氢化制备氨基萘磺酸的方法，所述催化剂包含新鲜的阮内镍催化剂和阮内镍催化剂的组合，已经用于以前的氢化或氢化。

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