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    Production of nabumetone or precursors thereof
    42.
    发明授权
    Production of nabumetone or precursors thereof 失效
    萘丁酮或其前体的生产

    公开(公告)号：US5907069A

    公开(公告)日：1999-05-25

    申请号：US9510

    申请日：1998-01-20

    Applicant: Brian F. Becnel ,  Mahmood Sabahi ,  Kevin J. Theriot

    Inventor： Brian F. Becnel ,  Mahmood Sabahi ,  Kevin J. Theriot

    IPC: B01J31/24 ,  B01J31/34 ,  C07B61/00 ,  C07C37/00 ,  C07C39/38 ,  C07C41/16 ,  C07C41/42 ,  C07C43/225 ,  C07C45/00 ,  C07C45/51 ,  C07C45/62 ,  C07C45/68 ,  C07C45/69 ,  C07C45/74 ,  C07C47/575 ,  C07C49/255 ,  C07C39/14 ,  C07C41/00 ,  C07C47/52

    CPC classification number: C07C49/255 ,  C07C37/00 ,  C07C41/16 ,  C07C41/34 ,  C07C41/40 ,  C07C41/42 ,  C07C45/004 ,  C07C45/512 ,  C07C45/62 ,  C07C45/68 ,  C07C45/74 ,  C07C47/575

    Abstract: In producing nabumetone or precursor thereof, use is made of 2-bromo-6-methoxynaphthalene formed by (a) methylating 6-bromo-2-naphthol with methyl bromide or methyl chloride, in a halogen-free liquid solvent comprising at least about 40% by weight of one or more compounds of the formula RZ where R is a hydrogen atom or an alkyl group, and Z is a hydroxyl group or a cyanide group with the proviso that if Z is a cyanide group, R is an alkyl group, and in the presence of at least one strong base; and (b) recovering and purifying 2-bromo-6-methoxynaphthalene so formed. The 6-bromo-2-naphthol in turn is preferably formed by reacting 1,6-dibromo-2-naphthol with hydrogen in a halogen-containing liquid solvent comprising at least about 50% by weight of (A) at least one liquid organic halide solvent in which the halogen content has an atomic number of 35 or less or (B) a mixture of water and at least one such liquid organic halide solvent, and in the presence of catalytic amounts of (i) a tungsten carbide-based catalyst, and (ii) at least one phase transfer catalyst, most preferably while purging HBr from the reaction mixture as it is formed. In this way, the quantities of by-products formed in the overall operation are reduced, the need for use of excess iron and/or dimethyl sulfate as reaction components is avoided, and the overall efficiency of plant operation is improved especially when conducted on a large scale.

    Abstract translation: 在制备萘布酮或其前体时，使用通过（a）在含卤素的液体溶剂中将6-溴-2-萘酚与甲基溴或甲基氯甲基化形成的2-溴-6-甲氧基萘，所述无卤液体溶剂包含至少约40 重量％的一种或多种式RZ化合物，其中R是氢原子或烷基，Z是羟基或氰基，条件是如果Z是氰基，则R是烷基， 并且在至少一个强碱的存在下; 和（b）回收和纯化如此形成的2-溴-6-甲氧基萘。 优选6-溴-2-萘酚通过在含卤素的液体溶剂中使1,6-二溴-2-萘酚与氢反应形成，该溶剂包含至少约50重量％的（A）至少一种液体有机物 卤素溶剂，其中卤素含量为35或更小的原子序数或（B）水和至少一种这样的液体有机卤化物溶剂的混合物，并且在催化量（i）碳化钨基催化剂 ，和（ii）至少一种相转移催化剂，最优选当其形成时从反应混合物中吹扫HBr。 以这种方式，减少了在整个操作中形成的副产物的数量，避免了使用过量的铁和/或硫酸二甲酯作为反应组分的需要，并且特别是当在 大规模

    Fungicidal spirocyclic amines
    43.
    发明授权
    Fungicidal spirocyclic amines 失效
    杀真菌的螺环胺

    公开(公告)号：US5849802A

    公开(公告)日：1998-12-15

    申请号：US722787

    申请日：1996-09-27

    Applicant: Waldemar Franz Augustin Pfrengle

    Inventor： Waldemar Franz Augustin Pfrengle

    IPC: A01N31/04 ,  A01N33/06 ,  A01N43/40 ,  A01N43/84 ,  C07C45/29 ,  C07C45/62 ,  C07C45/66 ,  C07C49/185 ,  C07C49/447 ,  C07C49/637 ,  C07C211/16 ,  C07C211/34 ,  C07C217/08 ,  C07C217/40 ,  A61K31/13 ,  A61K31/445 ,  A61K31/535 ,  C07C211/00

    CPC classification number: C07C217/40 ,  A01N31/04 ,  A01N33/06 ,  A01N43/40 ,  A01N43/84 ,  C07C211/16 ,  C07C211/34 ,  C07C217/08 ,  C07C45/29 ,  C07C45/62 ,  C07C45/66 ,  C07C49/185 ,  C07C49/447 ,  C07C49/637 ,  C07C2103/94

    Abstract: New antimicrobial spirocarbocyclic compounds are described, having the general formula I, ##STR1## or an acid-addition salt thereof, in which R.sub.1 represents an optionally substituted alkyl, cycloalkyl, cycloalkylalkyl, alkoxy, cycloalkoxy, alkoxyalkyl, aralkyl group R.sub.2 and R.sub.3 each independently represent hydrogen or an optionally substituted alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkylalkyl, bicycloalkyl, tricycloalkyl, alkoxyalkyl, aralkyl, aryl or haloaralkyl, a 4- to 6-membered heterocyclyl, tetrahydrofuryl or dioxolanyl group, or R.sub.2 and R.sub.3, together represents an optionally substituted, saturated or unsaturated chain which may optionally contain one or more oxygen atoms and which may optionally be aryl- or cycloalkyl-fused, and n represents zero or an integer from 1 to 3. The invention further relates to the preparation of the above spirocarbocyclic compounds, intermediates prepared during the synthesis of these compounds, compositions containing the compounds and their use as fungicides in the control of phytopathogenic fungi.

    Abstract translation: 描述了具有通式I，（I）或其酸加成盐的新型抗菌螺环碳环化合物，其中R 1表示任选取代的烷基，环烷基，环烷基烷基，烷氧基，环烷氧基，烷氧基烷基，芳烷基R2和 R 3各自独立地表示氢或任选取代的烷基，烯基，炔基，环烷基，环烷基烷基，二环烷基，三环烷基，烷氧基烷基，芳烷基，芳基或卤代烷基，4-至6-元杂环基，四氢呋喃基或二氧戊环基，或R 2和R 3， 一起表示任选取代的饱和或不饱和的链，其可任选地含有一个或多个氧原子，并且其可以任选地被芳基或环烷基稠合，并且n表示0或1至3的整数。本发明还涉及制备 的上述螺环化合物，在合成这些化合物期间制备的中间体，含有这些化合物的组合物及其用途 杀真菌剂控制植物病原真菌。

    Production of naphthyl-substituted ketones from naphthaldehydes
    44.
    发明授权
    Production of naphthyl-substituted ketones from naphthaldehydes 失效
    由萘醛生产萘基取代的酮

    公开(公告)号：US5847225A

    公开(公告)日：1998-12-08

    申请号：US846220

    申请日：1997-04-25

    Applicant: Venkataraman Ramachandran ,  Stephen E. Belmont

    Inventor： Venkataraman Ramachandran ,  Stephen E. Belmont

    IPC: C07C45/62 ,  C07C45/74 ,  C07C49/255 ,  C07C49/215

    CPC classification number: C07C49/255 ,  C07C45/62 ,  C07C45/74

    Abstract: A mixture formed from 2-naphthaldehyde (e.g., 6-methoxy-2-naphthaldehyde) and a dihydrocarbyl ketone having at least one hydrogen atom in the .alpha.-position (e.g., acetone) is heated in the presence of a heterogeneous basic catalyst (e.g., basic alumina) such that the unsaturated 2-naphthyl ketone is formed. The unsaturated ketone can be hydrogenated using, for example, a Pd/C catalyst to form the corresponding saturated ketone. The process enables efficient production of nabumetone and related pharmaceuticals by a clean reaction.

    Abstract translation: 将由2-萘甲醛（例如6-甲氧基-2-萘甲醛）和在α-位上具有至少一个氢原子的二烃基酮（例如丙酮）形成的混合物在非均相碱性催化剂（例如， ，碱性氧化铝），使得形成不饱和的2-萘基酮。 可以使用例如Pd / C催化剂氢化不饱和酮以形成相应的饱和酮。 该方法可以通过清洁反应有效地生产萘丁美酮和相关药物。

    Process for the preparation of 3,3,5-trimethylcyclohexanone
    46.
    发明授权
    Process for the preparation of 3,3,5-trimethylcyclohexanone 失效
    制备3,3,5-三甲基环己酮的方法

    公开(公告)号：US5728891A

    公开(公告)日：1998-03-17

    申请号：US668356

    申请日：1996-06-26

    Applicant: Wilfried Bueschken ,  Juergen Hummel

    Inventor： Wilfried Bueschken ,  Juergen Hummel

    IPC: B01J23/44 ,  C07B61/00 ,  C07C45/62 ,  C07C49/403 ,  C07C49/303

    CPC classification number: C07C45/62

    Abstract: A process for the preparation of 3,3,5-trimethylcyclohexanone by catalytic hydrogenation of isophorone, wherein the hydrogenation is carried out in a plurality of two or more series-connected loops, wherein each loop involves the use of one reactor, which comprises: (a) feeding isophorone and hydrogen to an upper part of a reactor to catalytically hydrogenate said isophorone to produce a hydrogenation product, (b) recycling a portion of said hydrogenation product back into said upper part of said reactor, (c) feeding the remainder of said hydrogenation product from said reactor to an upper part of a subsequent reactor wherein isophorone is catalytically hydrogenated to produce a subsequent hydrogenation product, and wherein a portion of said subsequent hydrogenation product has been recycled and is fed with said remainder of said hydrogenation product to said upper part of said subsequent reactor, (d) repeating step (c) until the subsequent reactor is the last reactor, (e) recovering the remainder of said subsequent hydrogenation product from said last reactor, and (f) obtaining 3,3,5-trimethylcyclohexanone from the product of step (e).

    Abstract translation: 通过异佛尔酮的催化氢化制备3,3,5-三甲基环己酮的方法，其中氢化在多个两个或更多个串联连接的环中进行，其中每个环包括使用一个反应器，其包含： （a）将异佛尔酮和氢气加入到反应器的上部以催化氢化所述异佛尔酮以产生氢化产物，（b）将所述氢化产物的一部分再循环回所述反应器的上部，（c） 的所述氢化产物从所述反应器到后续反应器的上部，其中异佛尔酮被催化氢化以产生随后的氢化产物，并且其中所述后续氢化产物的一部分已被再循环并与所述剩余的所述氢化产物一起加入 所述后续反应器的所述上部，（d）重复步骤（c），直到随后的反应器为最后的反应器，（e）回收t 剩余的来自所述最后一个反应器的所述随后的氢化产物，和（f）从步骤（e）的产物获得3,3,5-三甲基环己酮。

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