公开(公告)号：US4564704A

公开(公告)日：1986-01-14

申请号：US227552

申请日：1981-01-22

申请人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

发明人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

IPC分类号： C07C45/63 ,  C07C51/00 ,  C07C59/185 ,  C07C51/285 ,  C07C51/373

CPC分类号： C07C59/185 ,  C07C45/63 ,  C07C51/00

摘要： Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C. until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C. during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C., the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The product is a known compound suited for further syntheses.

摘要翻译： 通过将频倍他康酮引入两倍于氯的摩尔量来产生二氯可乐乐，最初冷却放热反应物质以保持温度低于约50℃，直到引入约60至80％的氯，然后加热反应物质 在导入剩余的氯的过程中温度高于50℃，从而产生二氯靛那烯，并且当反应物质的二氯新戊酮酮含量为至少约97％时终止氯引入。 将熔融产物加入到保持在至少约50℃温度的碱的水溶液中，碱的存在量是氯苯腈的摩尔量的三倍以上。 向所得到的3,3-二甲基-2-羟基 - 丁酸的盐溶液中加入大约9-12的pH，加入大约化学计量的高锰酸钾。 固体MnO 2析出并与3,3-二甲基-2-氧代 - 丁酸的基本上纯的溶解盐分离。 该产物是适用于进一步合成的已知化合物。

公开(公告)号：US4898974A

公开(公告)日：1990-02-06

申请号：US726218

申请日：1985-04-23

申请人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

发明人： Karlfried Dickore ,  Hans D. Engels ,  Hans Kratzer ,  Walter Merz

IPC分类号： C07C45/63 ,  C07C51/00 ,  C07C59/185

CPC分类号： C07C59/185 ,  C07C45/63 ,  C07C51/00

摘要： Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C. until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C. during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C., the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The produce is a known compound suited for further syntheses.

摘要翻译： 通过将频倍他康酮引入两倍于氯的摩尔量来产生二氯可乐乐，最初冷却放热反应物质以保持温度低于约50℃，直到引入约60至80％的氯，然后加热反应物质 在导入剩余的氯的过程中温度高于50℃，从而产生二氯一可乐酮，并且当反应物质的二氯新戊酮酮含量为至少约97％时终止氯引入。 将熔融产物加入到保持在至少约50℃温度的碱的水溶液中，碱的存在量是氯苯腈的摩尔量的三倍以上。 向所得到的3,3-二甲基-2-羟基 - 丁酸的盐溶液中加入大约9-12的pH，加入大约化学计量的高锰酸钾。 固体MnO 2析出并与3,3-二甲基-2-氧代 - 丁酸的基本上纯的溶解盐分离。 该产物是适用于进一步合成的已知化合物。

公开(公告)号：US4052460A

公开(公告)日：1977-10-04

申请号：US650651

申请日：1976-01-20

申请人： Karlfried Dickore ,  Hans Dieter Engels ,  Hans Kratzer ,  Walter Merz

发明人： Karlfried Dickore ,  Hans Dieter Engels ,  Hans Kratzer ,  Walter Merz

IPC分类号： C07C49/16 ,  C07C45/00 ,  C07C45/63 ,  C07C51/00 ,  C07C51/373 ,  C07C59/01 ,  C07C59/185 ,  C07C67/00

CPC分类号： C07C59/185 ,  C07C45/63 ,  C07C51/00

摘要： Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C, the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The product is a known compound suited for further syntheses.

公开(公告)号：US4035364A

公开(公告)日：1977-07-12

申请号：US708674

申请日：1976-07-26

申请人： Karlfried Dickore ,  Walter Merz ,  Johann Dahm ,  Donovan Norman Smith, Jr.

发明人： Karlfried Dickore ,  Walter Merz ,  Johann Dahm ,  Donovan Norman Smith, Jr.

IPC分类号： C07D253/075 ,  C07D253/06

CPC分类号： C07D253/075

摘要： In the methylation of 4-amino-6-t.-butyl-3-mercapto-1,2,4-triazin-5-one to produce 4-amino-6-t.-butyl-3-methylmercapto-1,2,4-triazine-5-one using methyl bromide, the reaction is run in the absence of air whereby product coloration is avoided. Desirably considerable agitation is employed along with recycle and especially with an emulsifying agent which markedly speeds up the reaction. Measures such as operating under a slight vacuum and recycle of unused methyl bromide and mother liquor are employed to improve the yield and to avoid the problems of discharging the bromides to the environment.

摘要翻译： 在4-氨基-6-叔丁基-3-巯基-1,2,4-三嗪-5-酮的甲基化中，得到4-氨基-6-叔丁基-3-甲基巯基-1,2 ，使用甲基溴的4-三嗪-5-酮，反应在不存在空气的情况下进行，由此避免产物着色。 特别是与循环使用相当大的搅拌，特别是使乳化剂显着加速反应。 使用诸如在轻微真空下操作和循环使用未使用的甲基溴和母液的措施来提高产量并避免将溴化物排放到环境中的问题。

公开(公告)号：US4151355A

公开(公告)日：1979-04-24

申请号：US904072

申请日：1978-05-08

申请人： Walter Merz

发明人： Walter Merz

IPC分类号： C07D253/075 ,  C07D253/06

CPC分类号： C07D253/075

摘要： 6-Tert.-butyl-3-mercapto-4-amino-1,2,4-triazin-(4H)-one is prepared by reacting pinacolone with a sulfur chloride at 0.degree. to 80.degree. C., optionally reacting the mixture with an aqueous amine solution, hydrolyzing the resulting product with an alkali metal hydroxide, heating the resulting mixture from 2 to 10 hours at 80.degree. to 150.degree. C., liberating a 3,3-dimethyl-2-oxo-butyric acid by acidifying with a mineral acid and reacting an aqueous solution of said 3,3-dimethyl-2-oxo-butyric acid with thiocarbohydrazide to yield the desired product.

摘要翻译： 6-加丁基-3-巯基-4-氨基-1,2,4-三嗪 - （4H） - 酮通过在0℃至80℃下使频哪酮与氯化硫反应制备，任选使该混合物 用胺水溶液，用碱金属氢氧化物水解所得产物，在80-150℃下将所得混合物加热2-10小时，通过酸化将3,3-二甲基-2-氧代 - 丁酸释放出来 与无机酸反应，并使所述3,3-二甲基-2-氧代 - 丁酸的水溶液与硫代碳酰肼反应，得到所需产物。

公开(公告)号：US4914095A

公开(公告)日：1990-04-03

申请号：US297228

申请日：1989-01-13

申请人： Walter Merz

发明人： Walter Merz

IPC分类号： C07D487/14 ,  A61K31/445 ,  A61K31/55 ,  A61P25/18 ,  A61P25/20

CPC分类号： A61K31/55

摘要： A compound of the formula ##STR1## is useful to treat psychotic disorders in humans, especially schizophrenia, and to prevent exacerbations thereof. The compound can be used as a single therapeutic agent or in combination with neuroleptics such as haloperidol.

摘要翻译： 式的化合物可用于治疗人类，特别是精神分裂症中的精神病，并防止其恶化。 该化合物可以用作单一治疗剂或与精神抑制药如氟哌啶醇组合使用。

公开(公告)号：US4615648A

公开(公告)日：1986-10-07

申请号：US177730

申请日：1980-08-13

申请人： Walter Merz

发明人： Walter Merz

IPC分类号： B65G53/52 ,  B65G53/58

CPC分类号： B65G53/521

摘要： Compressed air is introduced into a feed pipe system for transporting powdery or granular material in order to promote dense flow conditions. Variable or fixed size restrictions with decreasing size of blocking surface in the direction of the material flow equalize the amount of air entering the feed pipe along its entire length. The compressed air is introduced into the feed pipe through porous materials positioned at least in the region of the restrictions.

摘要翻译： 将压缩空气引入到用于输送粉末或颗粒材料的进料管系统中，以促进稠密流动条件。 在材料流动方向上阻塞表面的尺寸减小的可变或固定尺寸的限制使沿着其整个长度进入进料管的空气量相等。 压缩空气通过至少位于限制区域中的多孔材料引入进料管中。

公开(公告)号：US6034278A

公开(公告)日：2000-03-07

申请号：US194719

申请日：1998-12-17

申请人： Walter Merz ,  Martin Littmann ,  Udo Kraatz ,  Christoph Mannheims

发明人： Walter Merz ,  Martin Littmann ,  Udo Kraatz ,  Christoph Mannheims

IPC分类号： C07B53/00 ,  C07C209/88 ,  C07C211/27 ,  C07C211/29 ,  C07C209/00

CPC分类号： C07C209/88

摘要： The invention concerns a new method for producing optically active 1-phenylethylamines, wherein (a) racemic 1-phenylethylamines are reacted with (S)-(-)-N-phenylcarbamate lactic acid in the presence of an aliphatic or aromatic hydrocarbon and in the presence of a lower aliphatic alcohol, wherein the reaction components are measured so that for every mole of racemic amine, between 0.25 and 0.5 mole of (S)-(-)-N-phenylcarbamate lactic acid are present, the reaction mixture is then concentrated at a liquid-phase temperature of up to 40.degree. C., the resulting solid product is separated, treated with diluted, aqueous alkaline lye in the presence of a hydrocarbon, and the respective (R)-amine is isolated by distillation from the organic phase, and if necessary, (b) the mother liquor remaining after the separation of the solid product is reacted in the presence of a lower aliphatic alcohol with (S)-(-)-N-phenylcarbamate lactic acid, wherein the reaction components are measured so that the molar quantity of (S)-(-)-N-phenylcarbamate lactic acid is twice as great as the quantity of (R)-amine still remaining in the mother liquor, the reaction mixture is then concentrated at a liquid-phase temperature of up to 40.degree. C., the resulting solid product is separated and the (S)-amine is isolated by distillation from the mother liquor.

摘要翻译： PCT No.PCT / EP97 / 02988第 371日期1998年12月17日第 102（e）日期1998年12月17日PCT提交1997年6月9日PCT公布。 公开号WO97 / 49665 PCT 日期1997年12月31日本发明涉及一种用于制备光学活性1-苯基乙胺的新方法，其中（a）外消旋1-苯乙基胺与（S） - （ - ） - N-苯基氨基甲酸酯乳酸在脂肪族或 芳族烃和低级脂族醇的存在下，其中测量反应组分，使得对于每摩尔外消旋胺，存在0.25至0.5摩尔（S） - （ - ） - N-苯基氨基甲酸酯乳酸， 然后将反应混合物在高达40℃的液相温度下浓缩，分离得到的固体产物，在烃存在下用稀释的碱性碱水溶液处理，分离出（R） - 胺 （b）将固体产物分离后剩余的母液在低级脂族醇与（S） - （ - ） - N-苯基氨基甲酸酯乳酸的存在下反应， 其中测量反应组分 d，使得（S） - （ - ） - N-苯基氨基甲酸酯乳酸的摩尔量是母液中残留的（R） - 胺的量的两倍，然后将反应混合物以液 - 相温度高达40℃，分离得到的固体产物，并通过蒸馏从母液中分离出（S） - 胺。

公开(公告)号：US4812085A

公开(公告)日：1989-03-14

申请号：US815019

申请日：1985-12-30

申请人： Walter Merz

发明人： Walter Merz

IPC分类号： B65G53/20 ,  B65G53/18

CPC分类号： B65G53/20

摘要： A conduit for transporting finely-divided or fine-granular, dry bulk materials comprises a material conveyance zone and a zone for introducing the fluidizing medium separated from the first mentioned zone by a material which is permeable to gas and fluids. This conduit comprises at least one each of a closed feeder channel, a closed fluidizing channel and between these a fluidizing base. It runs approximately horizontal. In and/or above the fluidizing base are impeller nozzles with at least one outlet opening for a gaseous or fluid impeller medium. The fluidizing medium is introduced into the feeder channel/feeder channels at a positive pressure of 100-500 mm water column and the impeller medium at a positive pressure of 700-1500 mm water column.

摘要翻译： 用于运输细碎或细颗粒干燥散装材料的导管包括材料输送区和用于通过可渗透气体和流体的材料引入从第一所述区域分离的流化介质的区域。 该导管包括封闭的进料通道，封闭的流化通道中的至少一个，并且在这些流化基底之间。 它大致水平运行。 在流化基底内和/或上方是具有用于气态或流体叶轮介质的至少一个出口的叶轮喷嘴。 流化介质以100-500毫米水柱的正压力和叶轮介质在700-1500毫米水柱的正压下被引入进料通道/进料通道。

公开(公告)号：US4058526A

公开(公告)日：1977-11-15

申请号：US685234

申请日：1976-05-11

申请人： Walter Merz ,  Gunter Schummer

发明人： Walter Merz ,  Gunter Schummer

IPC分类号： C07D253/075 ,  C07D253/06

CPC分类号： C07D253/075

摘要： A process for the treatment of waste water obtained in the condensation of thiocarbohydrazide and an aqueous solution of an .alpha.-keto carboxylic acid such as, e.g., 3,3-dimethyl-2-oxo-butyric acid, which comprises mixing said waste water with a water-immiscible ketone, preferably selected from the group consisting of methyl isobutyl ketone, cyclohexanone and pinacolone, said ketone being employed in an amount sufficient to form two phases, separating said two phases, and discharging as waste the aqueous phase. Advantageously the pH of the waste water is no higher than about 6 and its temperature is 20.degree. to 50.degree. C. The organic phase comprises the ketone containing dissolved therein an adduct of the ketone with thiocarbohydrazide and/or similar amino materials originally present in waste water. The excess of the ketone may be recovered from the organic phase by distillation, or the organic phase may be treated with alkali to effect hydrolysis of such adducts, the ketone separated and recycled and the amino materials recovered.

摘要翻译： 一种用于处理硫代碳酰肼的缩合得到的废水和α-酮羧酸（例如3,3-二甲基-2-氧代 - 丁酸）的水溶液的方法，其包括将所述废水与 优选选自甲基异丁基酮，环己酮和频哪酮的水不混溶性酮，所述酮的用量足以形成两相，分离所述两相，并以废水的形式排出水相。 有利地，废水的pH不高于约6℃，其温度为20℃至50℃。有机相包含其中溶解有酮与硫代碳酰肼和/或最初存在于废物中的类似氨基物质的加合物的酮 水。 可以通过蒸馏从有机相中回收过量的酮，或者可以用碱处理有机相以进行这种加合物的水解，将酮分离并再循环并回收氨基物质。