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1. 发明申请

WO2008138856A1 IMPROVED PROCESS FOR WORKING UP DIACETONE ACRYLAMIDE SOLUTIONS FOR THE PREPARATION OF PURE DIACETONE ACRYLAMIDE 审中-公开
标题翻译：用于制备纯二胺酮丙烯酰胺的二胺酮丙烯酰胺溶液的改进方法
公开(公告)号：WO2008138856A1
公开(公告)日：2008-11-20
申请号：PCT/EP2008/055687
申请日：2008-05-08
申请人： DSM FINE CHEMICALS AUSTRIA NFG GMBH & CO KG , BRAUNE, Sascha , HOLUB, Bernhard , HUBER, Christoph
发明人： BRAUNE, Sascha , HOLUB, Bernhard , HUBER, Christoph
IPC分类号： C07C231/24 , C07C233/31
CPC分类号： C07C231/24 , C07C231/06 , C07C231/22 , C07C233/31
摘要： Improved process for working up diacetone acrylamide solutions, obtained by reaction of acetone or diacetone alcohol with acrylonitrile and sulfuric acid and subsequent dilution and neutralization, in which a) the organic phase obtained subsequent to the neutralization, which comprises the crude diacetone acrylamide, is hydrolyzed by addition of an aqueous alkaline solution in order to remove acrylamide, then b) after phase separation has been carried out, the organic phase, which comprises the crude diacetone acrylamide, is neutralized by addition of an acid, and c) in succession, low-boiling-point byproducts are removed by distillation in the presence of one or more polymerization inhibitors, then t-butylacrylamide is removed by distillation and, finally, the diacetone acrylamide is isolated by product distillation, and d) the diacetone acrylamide thus obtained is converted into its final form
摘要翻译：通过丙酮或双丙酮醇与丙烯腈和硫酸反应得到的丙酮丙烯酰胺溶液的改进方法，随后的稀释和中和，其中a）包含粗双丙酮丙烯酰胺的中和后获得的有机相被水解通过加入碱性水溶液以除去丙烯酰胺，然后b）进行相分离后，通过加入酸中和含有粗双丙酮丙烯酰胺的有机相，c）连续地低 - 沸点副产物在一种或多种聚合抑制剂存在下通过蒸馏除去，然后通过蒸馏除去叔丁基丙烯酰胺，最后通过产物蒸馏分离双丙酮丙烯酰胺，并且d）将由此获得的双丙酮丙烯酰胺转化进入其最终形式

2. 发明申请

WO2003084918A1 VERFAHREN ZUR HERSTELLUNG VON 2,2-DICHLORO-ODER DIBROMO-PHENYLESSIGSÄUREALKYLESTERN 审中-公开
标题翻译：用于生产2,2-二氯或二溴PHENYLESSIGSÄUREALKYLESTERN
公开(公告)号：WO2003084918A1
公开(公告)日：2003-10-16
申请号：PCT/EP2003/002407
申请日：2003-03-10
申请人： DSM FINE CHEMICALS AUSTRIA NFG GMBH & CO KG , KRICH, Sylvia , HOLUB, Bernhard
发明人： KRICH, Sylvia , HOLUB, Bernhard
IPC分类号： C07C67/22
CPC分类号： C07C67/22 , C07C69/65
摘要： Verbessertes Verfahren zur Herstellung von 2,2-Dichloro- oder Dibromophenylessigsäurealkylester der Formel in der X Cl oder Br ist, n eine ganze Zahl von 1 bis 5 sein kann, R Wasserstoff, C 1 C 8 -Alkyl, Aryl, Heteroaryl, C 1 -C 8 -Alkoxy, Aryloxy oder Halogen und R1 C 1 -C 8 -Alkyl bedeuten, bei welchem ein 2,2-Dichlor- oder Dibrom-phenylacetonitril der Formel in 0,8 bis 2 mol Wasser pro mol Nitril der Formel (II), 1 bis 8 mol Alkohol der Formel R1 OH (III), pro mol Nitril der Formel (II) und in Gegenwart von 1 bis 3 mol HCI oder HBr pro mol Nitril der Formel (II), gegebenenfalls in Anwesenheit eines unter den Reaktionsbedingungen inerten Lösungsmittels zu dem entsprechenden 2,2-Dichlorooder Dibromo-phenylessigsäurealkylester der Formel (I) umgesetzt wird, wobei die Reaktionstemperatur in der ersten Phase der Umsetzung bei 30 bis 60°C und in der zweiten Phase bei 60 bis 100°C liegt, worauf nach erfolgter Umsetzung das Reaktionsgemisch auf 20 bis 40°C abgekühlt und mit Wasser verdünnt wird, und der entsprechende 2,2-Dichloro- oder Dibromo-phenylessigsäurealkylester der Formel (I) isoliert wird.
摘要翻译：可以提高工艺的2,2-二氯或下式：其中X是Cl或Br的Dibromophenylessigsäurealkylester制备中，n是从1至5的整数，R为氢，C1C8烷基，芳基，杂芳基，C1C8烷氧基的意思是，芳氧基或卤素，且R 1的C 1 -C 8 - 烷基，其中在每摩尔式（II）的腈的摩尔为0.8〜2摩尔的水下式的2,2-二氯或二溴苯基乙腈，为1〜8摩尔的醇式的R1 OH（III），对于式（II）的腈的摩尔，在盐酸的1至3摩尔的存在或每个式（II）的腈的摩尔HBr的，任选地在惰性的存在下在反应条件下溶剂为相应的2-，式（I）的2- Dichlorooder二溴phenylessigsäurealkylester进行反应，反应温度是在30反应至60℃的第一阶段和在60至100℃的第二阶段，和反应后的反应混合物至20 冷却至40℃并用水稀释为t时，与相应的2,2-二氯或式（I）的二溴phenylessigsäurealkylester是分离的。

3. 发明授权

EP1490322B1 VERFAHREN ZUR HERSTELLUNG VON 2,2-DICHLORO- ODER DIBROMO-PHENYLESSIGSÄUREALKYLESTERN 有权
标题翻译：用于生产2,2-二氯或二溴PHENYLESSIGSÄUREALKYLESTERN
公开(公告)号：EP1490322B1
公开(公告)日：2015-07-29
申请号：EP03708200.5
申请日：2003-03-10
申请人： DSM Fine Chemicals Austria Nfg GmbH & Co KG
发明人： KRICH, Sylvia , HOLUB, Bernhard
IPC分类号： C07C67/22 , C07C69/65
CPC分类号： C07C67/22 , C07C69/65

4. 发明公开

EP2144869A1 IMPROVED PROCESS FOR WORKING UP DIACETONE ACRYLAMIDE SOLUTIONS FOR THE PREPARATION OF PURE DIACETONE ACRYLAMIDE 审中-公开
标题翻译：改进方法，治疗双丙酮丙烯酰胺的解决方案对于纯丙酮丙烯酰胺生产
公开(公告)号：EP2144869A1
公开(公告)日：2010-01-20
申请号：EP08759469.3
申请日：2008-05-08
申请人： DSM Fine Chemicals Austria Nfg GmbH & Co KG
发明人： BRAUNE, Sascha , HOLUB, Bernhard , HUBER, Christoph
IPC分类号： C07C231/24 , C07C233/31
CPC分类号： C07C231/24 , C07C231/06 , C07C231/22 , C07C233/31
摘要： Improved process for working up diacetone acrylamide solutions, obtained by reaction of acetone or diacetone alcohol with acrylonitrile and sulfuric acid and subsequent dilution and neutralization, in which a) the organic phase obtained subsequent to the neutralization, which comprises the crude diacetone acrylamide, is hydrolyzed by addition of an aqueous alkaline solution in order to remove acrylamide, then b) after phase separation has been carried out, the organic phase, which comprises the crude diacetone acrylamide, is neutralized by addition of an acid, and c) in succession, low-boiling-point byproducts are removed by distillation in the presence of one or more polymerization inhibitors, then t-butylacrylamide is removed by distillation and, finally, the diacetone acrylamide is isolated by product distillation, and d) the diacetone acrylamide thus obtained is converted into its final form.

5. 发明公开

EP1490322A1 VERFAHREN ZUR HERSTELLUNG VON 2,2-DICHLORO- ODER DIBROMO-PHENYLESSIGSÄUREALKYLESTERN 有权
标题翻译：用于生产2,2-二氯或二溴PHENYLESSIGSÄUREALKYLESTERN
公开(公告)号：EP1490322A1
公开(公告)日：2004-12-29
申请号：EP03708200.5
申请日：2003-03-10
申请人： DSM Fine Chemicals Austria Nfg GmbH & Co KG
发明人： KRICH, Sylvia , HOLUB, Bernhard
IPC分类号： C07C67/22 , C07C69/65
CPC分类号： C07C67/22 , C07C69/65
摘要： The invention relates to an improved method for producing 2,2-dichloro or dibromo-phenyl alkyl acetates of formula (1), in which X represents Cl or Br, n represents a whole number from 1 to 5, R represents hydrogen, C1-C8 alkyl, aryl, heteroaryl, C1-C8 alkoxy, aryloxy or halogen and R1 represents C1-C8 alkyl. According to said method, a 2,2-dichloro- or dibromo-phenylacetonitrile of formula (II) is reacted in 0.8 to 2 mol water per mol nitrile of formula (II), 1 to 8 mol alcohol of formula R1OH (III) per mol nitrile of formula (II) and in the presence of 1 to 3 mol HCl or HBr per mol nitrile of formula (II), optionally in the presence of a solvent that is inert in the reaction conditions, to form the corresponding 2,2-dichloro- or dibromo-phenyl alkyl acetates of formula (I), whereby the reaction temperature in the first phase lies between 30 and 60 °C and in the second phase between 60 and 100 °C. Once the reaction has taken place, the reaction mixture is cooled to between 20 and 40 °C, diluted with water and the 2,2-dichloro- or dibromo-phenyl alkyl acetate of formula (I) is isolated.

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