公开(公告)号：US20180093949A1

公开(公告)日：2018-04-05

申请号：US15562518

申请日：2015-06-04

申请人： ANTHEA AROMATICS PRIVATE LIMITED

发明人： Manoj Kumar MOHAPATRA ,  Ramamohanrao BENDAPUDI ,  Paul Vincent MENACHERRY ,  Vincent PAUL

IPC分类号： C07D201/06 ,  C07D201/16 ,  C07D227/087 ,  C01G9/02 ,  C01B21/14

CPC分类号： C07D201/06 ,  B01D3/36 ,  C01B21/14 ,  C01G9/02 ,  C07D201/04 ,  C07D201/16 ,  C07D227/087

摘要： Disclosed herein is an efficient, economical, industrially advantageous, straight-through process for the preparation of cyclic amides, also referred as lactams, in substantially pure form and high yield, from the corresponding cyclic ketones and a hydroxylammonium salt, using a combination of amphoteric metal oxide or amphoteric masked metal oxide and a base.

公开(公告)号：US20160221943A1

公开(公告)日：2016-08-04

申请号：US14917808

申请日：2014-07-07

申请人： TECHNIP ZIMMER GMBH

发明人： Andreas Bormann ,  Manfred Albrecht ,  Franz Samlitschka

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： A process for the recovery of ε-caprolactam from extract water of polycaprolactam obtained by hydrolytic polymerization, wherein the extract water is concentrated, subsequently contained oligomers are depolymerized, non-depolymerizable impurities are separated, water and low-boiling impurities are removed, wherein for adjusting the purity of the recovered ε-caprolactam and the energy consumption used for the process a part of the product is removed from the process as intermediate products.

摘要翻译： 从通过水解聚合获得的聚己内酰胺的萃取水中回收ε-己内酰胺的方法，其中提取水浓缩，随后包含的低聚物被解聚，不可解聚的杂质被分离，除去水和低沸点杂质，其中对于 调整回收的ε-己内酰胺的纯度和用于该方法的一部分产品所用的能量消耗作为中间产物。

公开(公告)号：US20140315972A1

公开(公告)日：2014-10-23

申请号：US14346445

申请日：2012-09-20

申请人： Valentina Ivanovna Akhapkina ,  Roman Vitalyevich Akhapkin

发明人： Valentina Ivanovna Akhapkina ,  Roman Vitalyevich Akhapkin

IPC分类号： C07D207/27 ,  G01N31/16

CPC分类号： G01N31/16 ,  A61K31/4015 ,  C07D201/16 ,  C07D201/18 ,  C07D207/27 ,  Y10T436/145555

摘要： The invention relates to a compound (RS)-2-(2-oxo-4-phenylpyrrolidin-1-yl)acetamide having modulatory activity with a commensurate effect, to a pharmaceutical substance (RS)-2-(2-oxo-4-phenylpyrrolidin-1-yl)acetamide containing: 2-(2-oxo-4-phenylpyrrolidin-1-yl)acetamide—no less than 99.0% and no more than 100.5% on dry basis, individual related impurities individually or in total—no more than 0.2%; residual amounts of organic solvents individually or in total—no more than 3000 ppm. The invention also relates to a method for producing the pharmaceutical substance differing in that the obtained raw materials are subjected to purification, crystallization and stabilization of the compound by processing it with demineralized (distilled) water, and the isothermal crystallization from propanol followed by drying. The invention also relates to compositions for internal and external application. The invention provides higher efficacy, safety, stability and width of therapeutic application. 55 cl, 3 dwg, 80 tbl, 27 ex.

摘要翻译： 本发明涉及具有相似作用的调节活性的化合物（RS）-2-（2-氧代-4-苯基吡咯烷-1-基）乙酰胺与药用物质（RS）-2-（2-氧代-4 - 2-（2-氧代-4-苯基吡咯烷-1-基）乙酰胺 - 不少于99.0％且不大于100.5％，单独或全部单独的相关杂质， 不超过0.2％; 剩余量的有机溶剂单独或总计不超过3000ppm。 本发明还涉及一种生产药物的方法，其不同之处在于，所得到的原料通过用软化（蒸馏）的水进行处理而进行化合物的纯化，结晶和稳定化，并用丙醇等温结晶，然后干燥。 本发明还涉及用于内部和外部应用的组合物。 本发明提供更高的疗效，安全性，稳定性和宽度的治疗应用。 55 cl，3 dwg，80 tbl，27 ex。

公开(公告)号：US20090088579A1

公开(公告)日：2009-04-02

申请号：US11918228

申请日：2006-04-07

申请人： Hideto Sugiura ,  Toru Inaoka ,  Shigeyuki Nozaki ,  Yoshihisa Oka

发明人： Hideto Sugiura ,  Toru Inaoka ,  Shigeyuki Nozaki ,  Yoshihisa Oka

IPC分类号： C07D207/267

CPC分类号： C07D207/267 ,  B01D9/0059 ,  C07D201/16

摘要： High-purity NVP can be produced by comprising at least two crystallization processes and supplying the mother liquor from the first crystallization process to the second crystallization process.Further, high-purity NVP can be obtained continuously and stably without plugging caused by depositing of crystals on the heat transfer surface of a crystallizer by controlling the water content in a feed NVP solution at the inlet of the crystallizer so as to be not lower than 0.7% by weight and not higher than 10% by weight.

摘要翻译： 可以通过包含至少两个结晶过程并将母液从第一结晶过程提供到第二结晶过程来生产高纯度NVP。 此外，通过控制结晶器入口处的进料NVP溶液中的水分含量，可以连续且稳定地获得高纯度NVP，而不会在结晶器的传热表面上沉积晶体而导致堵塞，从而不低于 0.7重量％且不高于10重量％。

公开(公告)号：US20080058513A1

公开(公告)日：2008-03-06

申请号：US11897883

申请日：2007-08-31

申请人： Chien-Hsien Li ,  Shou-Li Luo

发明人： Chien-Hsien Li ,  Shou-Li Luo

IPC分类号： C07D201/16

CPC分类号： C07D223/10 ,  C07D201/16

摘要： A system for purifying an aqueous solution of crude caprolactam is provided, which includes a filtration zone (A), an inspection unit (B), a purification zone (C), and a first temporary storage tank (D). The filtration zone (A) contains a filtration apparatus though which an aqueous solution of crude caprolactam is filtered to remove ionic impurities therein, so as to obtain caprolactam-containing filtrate; the inspection unit (B) is used for judging the filtrate from the filtration zone (A) meets the preset inspection standards; the purification zone(C) is used for concentrating and further purifying filtrate meeting the preset inspection standards, thereby forming a final caprolactam product; and the first temporary storage tank (D) is used for receiving the filtrate not meeting the preset inspection standards, which is then mixed with the aqueous solution of crude caprolactam and delivered back to the filtration zone (A).

摘要翻译： 提供了一种用于纯化粗己内酰胺水溶液的体系，其包括过滤区（A），检查单元（B），净化区（C）和第一临时储罐（D）。 过滤区（A）含有过滤装置，通过其过滤粗己内酰胺水溶液以除去其中的离子杂质，得到含己内酰胺的滤液; 检查单元（B）用于判断过滤区域（A）的滤液符合预设的检验标准; 净化区（C）用于浓缩并进一步净化满足预设检查标准的滤液，从而形成最终的己内酰胺产品; 并且第一临时储罐（D）用于接收不符合预设检查标准的滤液，然后将其与粗己内酰胺水溶液混合并输送到过滤区（A）。

公开(公告)号：US07238260B2

公开(公告)日：2007-07-03

申请号：US10973151

申请日：2004-10-26

申请人： Andrew P. Kahn ,  David W. Leyshon ,  Shaw-Chan Lin ,  Edward P. Carey

发明人： Andrew P. Kahn ,  David W. Leyshon ,  Shaw-Chan Lin ,  Edward P. Carey

IPC分类号： B01D3/14

CPC分类号： C07D207/26 ,  B01D3/14 ,  B01D3/146 ,  C07D201/16 ,  Y10S203/20

摘要： N-(2-hydroxyethyl)-2-pyrrolidone (HEP) is purified by a distillation sequence in which the purified HEP is recovered as a side stream without being separated as an overhead at any point in the procedure.

摘要翻译： 通过蒸馏顺序纯化N-（2-羟乙基）-2-吡咯烷酮（HEP），其中纯化的HEP作为侧流回收，而不在该过程的任何点被分离为塔顶馏出物。

公开(公告)号：US20060086602A1

公开(公告)日：2006-04-27

申请号：US10973151

申请日：2004-10-26

申请人： Andrew Kahn ,  David Leyshon ,  Shaw-Chan Lin

发明人： Andrew Kahn ,  David Leyshon ,  Shaw-Chan Lin

IPC分类号： B01D3/00

CPC分类号： C07D207/26 ,  B01D3/14 ,  B01D3/146 ,  C07D201/16 ,  Y10S203/20

摘要： N-(2-hydroxyethyl)-2-pyrrolidone (HEP) is purified by a distillation sequence in which the purified HEP is recovered as a side stream without being separated as an overhead at any point in the procedure.

摘要翻译： 通过蒸馏顺序纯化N-（2-羟乙基）-2-吡咯烷酮（HEP），其中纯化的HEP作为侧流回收而不在工序中的任何点被分离为塔顶馏出物。

公开(公告)号：US20040110943A1

公开(公告)日：2004-06-10

申请号：US10468263

申请日：2004-01-14

发明人： Maria Louisa Christina Dsinter-De Hondt ,  Joannes Albertus Wilhelmus Lemmens

IPC分类号： C07D201/16

CPC分类号： C07D201/16

摘要： Process for recovering caprolactam from a solution comprising caprolactam dissolved in an organic solvent, said process comprising: a) washing the solution with water or an aqueous alkaline solution, resulting in a washed solution comprising caprolactam and organic solvent and in a washing residue, b) evaporating organic solvent from the washed solution, resulting in caprolactam product, c) optionally, hydrogenating the caprolactam product, d) optionally, evaporating water from the caprolactam product, e) distilling the caprolactam product to recover caprolactam and a distillation residue, f) extracting the distillation residue with an organic solvent in the presence of water to obtain (i) an extract comprising caprolactam dissolved in organic solvent and (ii) an aqueous effluent, and g) recycling the extract to step a) or b).

摘要翻译： 从包含溶解在有机溶剂中的己内酰胺的溶液中回收己内酰胺的方法，所述方法包括：a）用水或碱性水溶液洗涤溶液，得到包含己内酰胺和有机溶剂的洗涤溶液，并在洗涤残渣中，b） 从洗涤的溶液中蒸发有机溶剂，得到己内酰胺产物，c）任选地使己内酰胺产物氢化，d）任选地从己内酰胺产物蒸发水，e）蒸馏己内酰胺产物以回收己内酰胺和蒸馏残渣，f） 在水存在下用有机溶剂蒸馏残余物，以获得（i）包含溶解在有机溶剂中的己内酰胺和（ii）含水流出物的提取物，和g）将提取物再循环到步骤a）或b）。

公开(公告)号：US20040014965A1

公开(公告)日：2004-01-22

申请号：US10296512

申请日：2003-07-30

发明人： Daniel Amoros ,  Philippe Leconte ,  Pierre Coqueret

IPC分类号： C07D21/08 ,  C07D21/16

CPC分类号： C07D201/16 ,  C07D201/08 ,  Y10S203/90

摘要： The invention concerns a method for purifying lactams, more particularly lactams obtained by cyclizing hydrolysis of aminonitrile. More particularly, the invention concerns the purification of null-caprolactam obtained by cyclizing hydrolysis of aminocapronitrile which consists in eliminating the ammonia from the reaction medium of the hydrolysis then in recuperating the lactam from said medium in purified form. Said recuperation is carried out by performing at least a distillation of the lactam in the presence of a base producing optionally a fronts fraction comprising compounds more volatile than the lactam, a fraction comprising the lactam to be recuperated to the degree of desired purity and a distillation tails comprising the lactam and compounds less volatile than the lactam. The distillation tails are treated by various processes such as evaporation in thin layers to recuperate the major part of the comprised caprolactam and recycling the latter in the purification process. The invention enables a high rate of recuperation of the caprolactam contained in the hydrolysis medium, while observing the required criteria of purity.

摘要翻译： 本发明涉及一种纯化内酰胺的方法，更特别的是通过环化氨基腈的水解得到的内酰胺。 更具体地说，本发明涉及通过环化氨基己腈的水解而得到的ε-己内酰胺的纯化，其包括从水解反应介质中除去氨，然后将内酰胺从纯化形式的所述培养基中回收。 所述的回收是通过在碱的存在下至少进行内酰胺的蒸馏来进行的，所述碱产生任选地含有比内酰胺更易挥发的化合物的前列馏分，包含待还原的内酰胺至所需纯度的馏分和蒸馏 尾部包含内酰胺和化合物比内酰胺更不易挥发。 蒸馏尾部通过各种方法处理，例如在薄层中蒸发以回收主要部分的己内酰胺并在净化过程中再循环。 本发明能够在观察所需的纯度标准的同时高效地回收水解介质中所含的己内酰胺。

公开(公告)号：US20030143146A1

公开(公告)日：2003-07-31

申请号：US10332585

申请日：2003-01-10

发明人： Hermann Luyken

IPC分类号： C01C001/00 ,  C07D201/16

CPC分类号： C07C231/24 ,  C07D201/16

摘要： A process is provided for the separation of ammonia (I) from mixtures (II) containing ammonia (I) and an amide (IV) selected from the group consisting of a lactam (IVa), an oligomer (IVb) and a polymer (IVc) with amide groups in the main chain, said amide (IV) having been obtained by reacting educts (III), selected from the group consisting of nitrites (IIIa), amines (IIIb), amino nitrites (IIIc) and amino amides (IIId), with water, wherein a) the educt (III) is reacted with water in the liquid phase, in the presence of an organic liquid diluent (V), to give a mixture (II) containing the amide (IV) and the ammonia (I), the diluent (V) exhibiting a miscibility gap with water under certain quantity, pressure and temperature conditions, b) the mixture (II) is converted under quantity, pressure and temperature conditions such that the diluent (V) and the water are in liquid form and exhibit a miscibility gap, to give a two-phase system consisting of a phase (VII) containing a higher proportion of diluent (V) than water, and a phase (VIII) containing a higher proportion of water than diluent (V), c) the phase (VII) is separated from the phase (VIII), d) all or part of the ammonia present in the phase (VII) is separated off by extraction (a) with a water-containing mixture (IX) to give an aqueous mixture (X) containing the ammonia which has been separated off, and a mixture (XI) containing less ammonia than the phase (VII), and e) the diluent (V), any residual ammonia and any by-products selected from the group consisting of low-boiling components, high-boiling components and unreacted compounds (III) are separated from the mixture (XI) to give the amide (IV).

摘要翻译： 提供了一种从含有氨（I）和选自内酰胺（IVa），低聚物（IVb）和聚合物（IVc）的酰胺（IV）的混合物（II）中分离氨（I）的方法 所述酰胺（IV）是通过使选自由亚硝酸盐（IIIa），胺（IIIb），氨基亚硝酸盐（IIIc）和氨基酰胺（IIId）组成的组的离析物（III）反应而获得的 ），其中a）在液相中，在有机液体稀释剂（V）的存在下，水解（III）与水反应，得到含有酰胺（IV）和氨的混合物（II） （I）中，稀释剂（V）在一定量，压力和温度条件下表现出与水的混溶性间隙，b）混合物（II）在数量，压力和温度条件下转化，使得稀释剂（V）和水 呈液态并显示混溶性间隙，得到由含有较高比例的相（VII）组成的两相体系 稀释剂（V）比水，和含有比稀释剂（V）更高比例的水的相（VIII），c）相（VII）从相（VIII）分离，d）全部或部分 通过用含水混合物（IX）萃取（a）分离相（VII）中存在的氨，得到含有已分离出的氨的含水混合物（X）和含有较少量的混合物（XI） （VII）中的氨，e）稀释剂（V），任选的残余氨和选自低沸点组分，高沸点组分和未反应化合物（III）的任何副产物与 混合物（Ⅺ），得到酰胺（Ⅳ）。