Method for producing ibuprofen
    12.
    发明授权
    Method for producing ibuprofen 失效
    生产布洛芬的方法

    公开(公告)号:US4981995A

    公开(公告)日:1991-01-01

    申请号:US500645

    申请日:1990-03-28

    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。

    Process for preparing vinylphenol polymers and copolymers
    14.
    发明授权
    Process for preparing vinylphenol polymers and copolymers 失效
    制备乙烯基苯酚聚合物和共聚物的方法

    公开(公告)号:US5453481A

    公开(公告)日:1995-09-26

    申请号:US406351

    申请日:1995-03-01

    摘要: The present invention provides a unique and novel way of producing polyhydroxystyrene which comprises the steps of (a) heating 4-hydroxyacetophenone under suitable hydrogenation conditions of temperature and pressure in the presence of a suitable palladium catalyst and for a sufficient period of time to form 4-hydroxyphenylmethylcarbinol; (b) heating 4-hydroxyphenylmethylcarbinol under suitable conditions of temperature and pressure and for a sufficient period of time to form said polyhydroxystyrene.

    摘要翻译: 本发明提供了一种独特且新颖的多羟基苯乙烯生产方法,该方法包括以下步骤:(a)在合适的钯催化剂存在下,在合适的温度和压力的氢化条件下加热4-羟基苯乙酮,并持续足够的时间以形成4 - 羟基苯基甲基甲醇 (b)在合适的温度和压力条件下加热4-羟基苯基甲基甲醇并持续足够的时间以形成所述多羟基苯乙烯。

    Process for preparing
.alpha.-chloro-.alpha.-oximino-4-hydroxyacetophenone
    15.
    发明授权
    Process for preparing .alpha.-chloro-.alpha.-oximino-4-hydroxyacetophenone 失效
    制备α-氯-α-肟基-4-羟基苯乙酮的方法

    公开(公告)号:US5292945A

    公开(公告)日:1994-03-08

    申请号:US17550

    申请日:1993-02-16

    IPC分类号: C07C259/02 C07C53/00

    CPC分类号: C07C259/02

    摘要: A process for the preparation of .alpha.-chloro-.alpha.-oximino-4-hydroxyacetophenone by reacting nitrosyl chloride with a mixture of 4-hydroxyacetophenone and a strong acid catalyst such as hydrogen chloride is disclosed. The nitrosyl chloride is introduced as a gas into the reactor to contact 4-hydroxyacetophenone and said acid catalyst dissolved in a solvent therein.

    摘要翻译: 公开了通过使亚硝酰氯与4-羟基苯乙酮和强酸催化剂如氯化氢的混合物反应来制备α-氯-α-肟基-4-羟基苯乙酮的方法。 将亚硝酰氯作为气体引入反应器中以接触溶于其中的溶剂中的4-羟基苯乙酮和所述酸催化剂。