公开(公告)号：US5151551A

公开(公告)日：1992-09-29

申请号：US579427

申请日：1990-09-06

申请人： Edward G. Zey ,  Thomas H. Shockley ,  Debra A. Ryan ,  Gary L. Moss

发明人： Edward G. Zey ,  Thomas H. Shockley ,  Debra A. Ryan ,  Gary L. Moss

IPC分类号： C07C51/43

CPC分类号： C07C51/43

摘要： This invention pertains to a method of purifying ibuprofen-comprising reaction product mixtures. The method of purification is based on crystallization of ibuprofen from a hydrocarbon solvent and the discovery that there are impurity complexes in the ibuprofen-comprising reaction product mixtures which cannot be removed by crystallization from a hydrocarbon solvent.The method of the invention includes at least one step in which the impurity complex in a first ibuprofen-comprising mixture is destabilized or broken up, followed by crystallization of the ibuprofen from a second solution or mixture comprising the first ibuprofen-comprising mixture, whereby the impurities which were previously complexed can then be removed from the ibuprofen by the crystallization of ibuprofen from a solvent.

公开(公告)号：US4981995A

公开(公告)日：1991-01-01

申请号：US500645

申请日：1990-03-28

申请人： Varadaraj Elango ,  Mark A. Murphy ,  Brad L. Smith ,  Kenneth G. Davenport ,  Graham N. Mott ,  Edward G. Zey ,  Gary L. Moss

发明人： Varadaraj Elango ,  Mark A. Murphy ,  Brad L. Smith ,  Kenneth G. Davenport ,  Graham N. Mott ,  Edward G. Zey ,  Gary L. Moss

IPC分类号： B01J31/24 ,  C07C45/46 ,  C07C51/12 ,  C07C57/30

CPC分类号： B01J31/2404 ,  B01J31/24 ,  C07C45/46 ,  C07C51/12 ,  B01J2231/34 ,  B01J2531/824 ,  Y02P20/584

摘要： A method is provided for the preparation of ibuprofen by carbonylating 1-(4'-isobutylphenyl)ethanol (IBPE) with carbon monoxide in an acidic aqueous medium, e.g. containing at least 10% of water based on the weight of IBPE initially added, at a temperature of at least about 10.degree. C. and a carbon monoxide pressure of at least about 500 psig, and in the presence of (1) a catalyst complex consisting essentially of a palladium compound in which the palladium has a valence of zero to 2 and is complexed with at least one monodentate phosphine ligand miscible with the organic phase of the reaction medium, the phosphorus/palladium mole ratio in said palladium compound and ligand being at least about 2:1 when the palladium/IBPE mole ratio is such that palladium=1 and IBPE=10,000 or more; (2) dissociated hydrogen ions from an acid which is substantially completely ionizable in dilute aqueous solution such that the mole ratio of hydrogen ions to IBPE added to the reaction zone is at least about 0.15; and, (3) dissociated halide ions such that the mole ratio of halide ions to IBPE added to the reaction zone is at least about 0.15. Advantageously, a hydrogen halide is the source of hydrogen ions and halide ions. The carbonylation is preferably integrated with a method of producing IBPE from isobutylbenzene wherein the latter compound is subjected to Friedel-Crafts reaction with an acetylating agent to produce 4-isobutylacetophenone, which is then reduced with hydrogen in the presence of a hydrogenation catalyst, or with a reducing agent containing available hydrogen, to obtain IBPE. The palladium catalyst complex can be precipitated from an organic phase of the carbonylation reaction which typically includes the ibuprofen product. The precipitated catalyst complex can be recycled without further treatment.

摘要翻译： 提供了一种通过在酸性水性介质中将1-（4'-异丁基苯基）乙醇（IBPE）与一氧化碳羰基化来制备布洛芬的方法，例如， 在至少约10℃的温度和至少约500psig的一氧化碳压力下，在（1）催化剂络合物的存在下，基于最初加入的IBPE的重量，含有至少10％的水 基本上由钯化合物组成，其中钯的价数为0至2，并且与至少一种与反应介质的有机相可混溶的单齿膦配体络合，所述钯化合物和配体中的磷/钯摩尔比为 当钯/ IBPE摩尔比使得钯= 1和IBPE = 10,000或更高时，至少约2:1; （2）从在稀水溶液中基本完全可离子化的酸离解氢离子使得加入到反应区中的氢离子与IBPE的摩尔比至少为约0.15; 和（3）离解的卤离子使得加入反应区的卤离子与IBPE的摩尔比至少为约0.15。 有利地，卤化氢是氢离子和卤离子的来源。 羰基化优选与从异丁基苯生产IBPE的方法相结合，其中后一种化合物与乙酰化剂进行Friedel-Crafts反应以产生4-异丁基苯乙酮，然后在氢化催化剂存在下用氢还原，或与 含有可用氢的还原剂，以获得IBPE。 钯催化剂络合物可以从通常包括布洛芬产物的羰基化反应的有机相中沉淀出来。 沉淀的催化剂络合物可以循环使用，无需进一步处理。

公开(公告)号：US5271811A

公开(公告)日：1993-12-21

申请号：US15270

申请日：1993-02-08

申请人： Siegbert Rittner ,  Adolf Schmidt ,  Larry O. Wheeler ,  Gary L. Moss ,  Edward G. Zey

发明人： Siegbert Rittner ,  Adolf Schmidt ,  Larry O. Wheeler ,  Gary L. Moss ,  Edward G. Zey

IPC分类号： C07C51/44 ,  B01D3/10

CPC分类号： C07C51/44

摘要： 2-(4-Isobutylphenyl)-propionic acid is purified by subjecting it to a vacuum rectification, in which the temperature is below the decomposition temperature of the acid.

摘要翻译： 2-（4-异丁基苯基） - 丙酸通过进行真空精馏而纯化，其中温度低于酸的分解温度。