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    PROCESS FOR PREPARING 1,1-DISUBSTITUTED ETHYLENE MONOMERS
    3.
    发明申请
    PROCESS FOR PREPARING 1,1-DISUBSTITUTED ETHYLENE MONOMERS 审中-公开
    制备1,1-取代的乙烯单体的方法

    公开(公告)号：WO2015150882A1

    公开(公告)日：2015-10-08

    申请号：PCT/IB2014/064144

    申请日：2014-08-29

    申请人： AFINITICA TECHNOLOGIES, S. L.

    发明人： TCHAPLINSKI, Vladimir ,  GHERARDI, Stefano ,  DE LA FUENTE MOLINA, Verónica

    IPC分类号： C07C67/347 ,  C07C253/30 ,  C07F7/08 ,  C07D307/12

    CPC分类号： C07C253/30 ,  C07C67/343 ,  C07C2601/14 ,  C07C2601/16 ,  C07D307/12 ,  C07F7/0818 ,  C07C255/23 ,  C07C69/593

    摘要： Process for preparing 1,1-disubstituted ethylene monomers The present invention relates to a process for preparing 1,1-disubstituted ethylene monomers having general formula (I) from a compound of general formula (II) and an active methylene compound of general formula (III) using a catalytic amount of an ammonium or iminium salt in homogeneous phase or supported on a solid substrate. Said process allows the direct synthesis of the monomers and finds application in the preparation of a wide variety of monomers. The products obtained are reactive monomers of high purity which find application in the field of fast curing adhesives.

    摘要翻译： 制备1,1-双取代乙烯单体的方法本发明涉及由通式（II）的化合物和通式（II）的活性亚甲基化合物制备具有通式（I）的1,1-二取代乙烯单体的方法， III）使用催化量的均匀相中的铵或亚铵盐或负载在固体基质上。 所述方法允许单体的直接合成，并且可用于制备多种单体。 所得产物是高纯度的反应性单体，可用于快速固化粘合剂领域。

    PROCESS FOR THE MANUFACTURE OF AN AMINO ESTER
    4.
    发明申请
    PROCESS FOR THE MANUFACTURE OF AN AMINO ESTER 审中-公开
    氨基酸制备方法

    公开(公告)号：WO2015071500A1

    公开(公告)日：2015-05-21

    申请号：PCT/EP2014/074942

    申请日：2014-11-18

    申请人： RHODIA OPERATIONS

    发明人： MARION, Philippe ,  MORVAN, Didier

    IPC分类号： C07C227/04 ,  C07C253/30

    CPC分类号： C07C227/04 ,  C07C253/30 ,  C08G69/44 ,  C07C255/23 ,  C07C229/08

    摘要： Process for the manufacture of an amino ester of formula (I) R 1 -O-C(O)-(CH 2 ) n -NH 2 (I) in which n is an integer from 10 to 15 from an unsaturated ester responding to formula (II) R 1 -O-C(O)-(CH 2 ) m -CH=CH-R 2 (II) in which R 1 is either H or a saturated alkyl group containing from 1 to 5 carbon atoms; R 2 is either H or an alkyl group containing from 1 to 10 carbon atoms, either saturated or containing 1 or 2 unsaturations and bearing optionally a hydroxyl, a carboxylic or an ester group, and m is equal to 7, 8, 9, 10 or 11; said process comprising: submitting the unsaturated ester of formula (II) to a catalytic cross-metathesis reaction with a pentenenitrile chosen among 2-pentenenitrile or 3-pentenenitrile in order to obtain a ester-nitrile responding to formula (III) R 1 -O-C(O)-(CH 2 ) m -CH=CH-(CH 2 ) p -CN (III) in which m is equal to 7, 8, 9, 10 or 11 and p is equal to 0 or 1, and submitting the obtained ester-nitrile of formula (III) to an hydrogenation in order to obtain the amino ester of formula (I).

    摘要翻译： 制备式（I）的氨基酯的方法R1-OC（O） - （CH2）n-NH2（Ⅰ），其中n为响应式（Ⅱ）的不饱和酯的10至15的整数R1 -OC（O） - （CH 2）m -CH = CH-R 2（II），其中R 1是H或含有1至5个碳原子的饱和烷基; R 2是H或含有1至10个碳原子的烷基，其为饱和的或含有1或2个不饱和基团，并且任选具有羟基，羧基或酯基，m等于7,8,9,10或 11; 所述方法包括：将式（II）的不饱和酯与选自2-戊烯腈或3-戊烯腈的戊烯腈进行催化交叉复分解反应，以获得响应式（III）的酯腈R1-OC（ O） - （CH 2）m -CH = CH-（CH 2）p -CN（III），其中m等于7,8,9,10或11，p等于0或1，并将所得酯 （III）的腈与氢化反应，得到式（I）的氨基酯。

    A PROCESS FOR THE PREPARATION OF PREGABALIN
    6.
    发明申请
    A PROCESS FOR THE PREPARATION OF PREGABALIN 审中-公开
    一种制备PREGABALIN的方法

    公开(公告)号：WO2014072785A8

    公开(公告)日：2014-09-18

    申请号：PCT/IB2013002435

    申请日：2013-11-04

    申请人： HIKAL LTD

    发明人： MOHILE SWAPNIL SURENDRA ,  YERANDE SWAPNIL GULABRAO ,  LUNGE SARIKA MADHUKARRAO ,  PATEL RAMESHKUMAR MAGHABHAI ,  GUGALE SHIVAJI BALBHIM ,  THAKUR RAJESH MATAPRASAD ,  MOKAL RAMESH ANANDA ,  GANGOPADHYAY ASHOK KUMAR ,  NIGHTINGALE PETER DAVID

    IPC分类号： A61K31/197 ,  C07C229/08 ,  C07C229/24

    CPC分类号： C12P13/001 ,  C07C227/04 ,  C07C227/30 ,  C07C253/10 ,  C07C253/30 ,  C12P13/002 ,  C12P41/005 ,  C07C255/23 ,  C07C255/09 ,  C07C255/19 ,  C07C229/08

    摘要： The present invention provides an improved process for the preparation of a compound of formula (I), which comprises the steps of: formula (I), (a) reacting isovaleraldehyde of formula (II) and alkyl cyanoacetate of formula (III) optionally in presence of salts of weak acid and weak base or weak base in a suitable solvent to get 2-cyano-5- methyl-hex-2-enoic acid alkyl ester of formula (IV); (b) reacting 2-cyano-5-methyl-hex-2-enoic acid alkyl ester of formula (IV) with a suitable cyanide source in water or in an organic solvent or mixture thereof to get 2-isobutylsuccinonitrile of formula (V); (c) obtaining optionally 2-isobutylsuccinonitrile of formula (V) by reacting isovaleraldehyde of formula (II) and alkyl cyanoacetate of formula (III) in presence of suitable cyanide source in water or in an organic solvent or mixture thereof in single step; (d) converting 2-isobutylsuccinonitrile of formula (V) to racemic 3-cyano-5-methyl-hexanoic acid or salt thereof of formula (VI) with a genetically modified nitrilase enzyme (Nit 9N_56_2) in water or optionally with an organic co-solvent at appropriate pH and temperature; (e) converting racemic 3-cyano-5-methyl-hexanoic acid or salt thereof of formula (VI) to racemic alkyl 3-cyano-5-methyl-hexanoate of formula (VII) by treatment with alcohol (R3OH) and acidic catalyst or alkyl halide (R3X) in presence of a base in a suitable solvent or a mixture of solvents thereof;.(f) obtaining (S)-alkyl 3 -cyano-5 -methyl -hexanoate of formula (VIII) and (R)-3-cyano-5-methyl- hexanoic acid or salt thereof of formula (X) by enzymatic enantioselective hydrolysis in water or organic solvent or a mixture thereof from racemic alkyl 3-cyano-5-methyl-hexanoate of formula (VII);.(g) obtaining optionally the compound of formula (VII) by racemizing unwanted (R)-3-cyano-5- methyl-hexanoic acid or salt thereof of formula (X) or substantially enriched (R)-3 -cyano-5 - methyl-hexanoic acid salt thereof of formula (X) in presence of a base in organic solvent or a mixture thereof; (h) converting (S)-alkyl 3-cyano-5-methyl-hexanoate of formula (VIII) to pregabalin of formula (I) by hydrolyzing ester group with suitable alkali or alkaline earth metal base followed by hydrogenation optionally in one pot in a solvent selected from water or other organic solvents or a mixture thereof in presence of a suitable hydrogenation catalyst.

    摘要翻译： 本发明提供了制备式（I）化合物的改进方法，其包括以下步骤：式（I），（a）使式（II）的异戊醛和式（III）的氰基乙酸烷基酯任选地 在合适的溶剂中存在弱酸和弱碱或弱碱的盐以得到式（IV）的2-氰基-5-甲基 - 己-2-烯酸烷基酯; （b）使式（IV）的2-氰基-5-甲基 - 己-2-烯酸烷基酯与合适的氰化物源在水或有机溶剂或其混合物中反应以得到式（V）的2-异丁基琥珀腈， ; （c）通过使式（II）的异戊醛和式（III）的氰基乙酸烷基酯在合适的氰化物源存在下在水中或在有机溶剂或其混合物中单步反应获得式（V）的2-异丁基丁二腈; （d）将式（V）的2-异丁基丁二腈转化为式（VI）的外消旋3-氰基-5-甲基 - 己酸或其盐与基因改造的腈水解酶（Nit 9N_56_2）在水中或任选与有机共聚物 - 在适当的pH和温度下的溶剂; （e）通过用醇（R 3 OH）和酸性催化剂处理将式（VI）的外消旋3-氰基-5-甲基 - 己酸或其盐转化为式（VII）的3-氰基-5-甲基 - 己酸外消旋烷基酯 或烷基卤化物（R3X）在碱的存在下在合适的溶剂或其溶剂混合物中反应;（f）获得式（VIII）和（R）的（S） - 烷基-3-氰基-5-甲基 - （X）的3-氰基-5-甲基 - 己酸或其盐通过在水或有机溶剂或其混合物中的酶对映选择性水解由式（VII）的3-氰基-5-甲基 - 己酸外消旋烷基酯制备。 （g）通过外消旋式（X）的不需要的（R）-3-氰基-5-甲基 - 己酸或其盐或基本上富集的（R）-3-氰基-5 - 式（X）的甲基 - 己酸盐在碱存在下在有机溶剂或其混合物中反应; （h）通过用合适的碱金属或碱土金属碱水解酯基团，然后任选地在一锅中将式（VIII）的3-氰基-5-甲基 - 己酸（S） - 烷基酯转化成式（I）的普瑞巴林 选自水或其它有机溶剂或其混合物的溶剂，在合适的氢化催化剂存在下进行。

    ALPHA-CYANOACRYLATE ESTER SYNTHESIS
    8.
    发明申请
    ALPHA-CYANOACRYLATE ESTER SYNTHESIS 审中-公开
    ALPHA-氰基丙烯酸酯合成

    公开(公告)号：WO2012041395A1

    公开(公告)日：2012-04-05

    申请号：PCT/EP2010/064692

    申请日：2010-10-01

    申请人： LOCTITE (R & D) LIMITED ,  HYNES, Stephen

    发明人： HYNES, Stephen

    IPC分类号： C07C253/30 ,  C07C255/23

    CPC分类号： C07C253/30 ,  C07C255/23

    摘要： The high temperatures required for cracking the cyanoacrylate oligomers, produced by the Knovenagel condensation of formaldehyde and a cyanoacetate, limit the synthetic diversity and the number of different side chains that can be incorporated into a cyanoacrylate prepared using this method. Accordingly, the diversity of cyanoacrylate monomers prepared industrially is quite limited. Disclosed herein is a method for the preparation of alpha-Cyanoacrylate ester monomers from a variety of phosphonium and ammonium alpha-cyanoacrylate salts. The phosphonium and ammonium alpha-cyanoacrylate salts are of the general formula: (I).

    摘要翻译： 通过甲醛和氰基乙酸酯的Knovenagel缩合产生的氰基丙烯酸酯低聚物裂解所需的高温限制了可以掺入使用该方法制备的氰基丙烯酸酯中的不同侧链的合成多样性和数量。 因此，工业上制备的氰基丙烯酸酯单体的多样性是非常有限的。 本文公开了一种从各种鏻和α-氰基丙烯酸铵盐制备α-氰基丙烯酸酯单体的方法。 鏻和α-氰基丙烯酸铵盐具有以下通式：（I）。