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    PREPARATION METHOD OF 3,7,11-TRIMETHYLDODEC-2,4,6,10-TETRAENE-1-YL PHOSPHONIC SALT
    2.
    发明授权
    PREPARATION METHOD OF 3,7,11-TRIMETHYLDODEC-2,4,6,10-TETRAENE-1-YL PHOSPHONIC SALT 有权
    HERSTELLUNGSVERFAHRENFÜR3,7,11-TRIMETHYLDODEC-2,4,6,10-TETRAEN-1-YL-PHOSPHONSALZ

    公开(公告)号：EP2799440B1

    公开(公告)日：2017-05-24

    申请号：EP12861708.1

    申请日：2012-12-10

    申请人： Nanjing University Of Technology ,  Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory

    发明人： LV, Chunlei ,  PI, Shiqing ,  CHEN, Jianhui ,  LU, Dingqiang ,  OUYANG, Pingkai

    IPC分类号： C07F9/54

    CPC分类号： C07F9/5442 ,  C07F9/5428

    摘要： Provided in the present invention is a preparation method for a phosphonic salt, comprising the step of: reacting 3,7,11-trimethyldodec-1,4,6,10-tetraene-3-ol with triarylphosphine and an acid in an alcohol solvent at 50-100°C to form the phosphonic salt, wherein the acid is a sulfamic acid or methanesulfonic acid, and the alcohol solvent is a straight chain monohydric alcohol containing 1-5 carbon atoms. The method is performed in nearly neutral conditions, greatly reducing the generation of impurities and greatly obtaining phosphonic salt with an increased E content. The yield of lycopene obtained by using the phosphonic salt as a raw material is high.

    摘要翻译： 本发明提供了一种膦酸盐的制备方法，包括以下步骤：使3,7,11-三甲基十二烷-1,4,6,10-四烯-3-醇与三芳基膦和酸在醇溶剂中反应 在50-100℃下形成膦酸盐，其中酸是氨基磺酸或甲磺酸，醇溶剂是含有1-5个碳原子的直链一元醇。 该方法在几乎中立的条件下进行，大大减少了杂质的产生，并大大地获得了具有增加的E含量的膦酸盐。 通过使用膦酸盐作为原料获得的番茄红素的产率高。

    METHOD FOR SYNTHESIZING 2,7-DIMETHYL-2,4,6-OCTATRIENE-1,8-DIALDEHYDE
    4.
    发明公开
    METHOD FOR SYNTHESIZING 2,7-DIMETHYL-2,4,6-OCTATRIENE-1,8-DIALDEHYDE 有权
    VERFAHREN ZUR SYNTHESE VON 2,7-二甲基-2,4,6-OCTATRIEN-1,8-DIALDEHYD

    公开(公告)号：EP2799420A1

    公开(公告)日：2014-11-05

    申请号：EP12863035.7

    申请日：2012-12-10

    申请人： Nanjing University Of Technology ,  Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory

    发明人： CHEN, Jianhui ,  LV, Chunlei ,  PI, Shiqing ,  LU, Dingqiang ,  OUYANG, Pingkai

    IPC分类号： C07C45/52 ,  C07C47/21

    CPC分类号： C07C45/42 ,  C07C1/324 ,  C07C41/06 ,  C07C41/18 ,  C07C41/22 ,  C07C45/52 ,  C07F9/38 ,  C07C47/21

    摘要： Provided in the present invention is a method for synthesizing 2,7-dimethyl-2,4,6-octatriene-1,8-dialdehyde. The synthesis method comprises the following steps: (1) adding acetaldehyde diethyl acetal and ethyl-(1-propenyl)-ether under the effect of a catalyst to produce 1,1,3-triethoxy-2-methyl-butane; (2) pyrolysis synthesizing 1,1,3-triethoxy-2-methyl-butane under the catalytic effects of isoquinoline and p-Toluenesulfonic acid to produce 1-methoxy-2-methyl-1,3-butadiene; (3) dissolving 1-methoxy-2-methyl-1,3-butadiene in anhydrous ethanol solvent for synthesis with a phase transfer catalyst, cetyl-trimethyl ammonium bromide, and a chlorinating agent, trichloroisocyanuric acid, to generate 4,4-diethoxy-3-methyl-1- chloro-butene; (4) combining 4,4-diethoxy-3-methyl-1-chloro-butene with a triphenylphosphine salt to produce a phosphonium salt; and (5) condensing the phosphonium salt under the effects of hydrogen peroxide in conjunction with sodium carbonate solution to generate 1,1,8,8-tetramethyl-2,7-dimethyl-2,4,6-octatriene; then hydrolyzing under acidic conditions to synthesize 2,7-dimethyl-2,4,6-octatriene-1,8- dialdehyde. The present invention has a simple process route, is easy to operate, and has mild conditions, great yield, and great industrial value.

    摘要翻译： 本发明提供了合成2,7-二甲基-2,4,6-辛二烯-1,8-二醛的方法。 合成方法包括以下步骤：（1）在催化剂作用下加入乙醛缩二乙醇和乙基（1-丙烯基） - 醚，制得1,1,3-三乙氧基-2-甲基 - 丁烷; （2）在异喹啉和对甲苯磺酸的催化作用下热解合成1,1,3-三乙氧基-2-甲基 - 丁烷，得到1-甲氧基-2-甲基-1,3-丁二烯; （3）将1-甲氧基-2-甲基-1,3-丁二烯溶于无水乙醇溶剂中，用相转移催化剂，十六烷基三甲基溴化铵和氯化剂三氯异氰脲酸合成，得到4,4-二乙氧基 -3-甲基-1-氯 - 丁烯; （4）将4,4-二乙氧基-3-甲基-1-氯 - 丁烯与三苯基膦盐结合以产生鏻盐; 和（5）在过氧化氢与碳酸钠溶液的作用下将鏻盐缩合，生成1,1,8,8-四甲基-2,7-二甲基-2,4,6-辛三烯; 然后在酸性条件下水解合成2,7-二甲基-2,4,6-辛二烯-1,8-二醛。 本发明工艺路线简单，操作方便，条件温和，产量大，工业价值高。

    PREPARATION METHOD OF LYCOPENE INTERMEDIATE 3-METHYL-4,4-DIALKOXY-1-BUTALDEHYDE
    5.
    发明公开
    PREPARATION METHOD OF LYCOPENE INTERMEDIATE 3-METHYL-4,4-DIALKOXY-1-BUTALDEHYDE 有权
    VERFAHREN ZUR HERSTELLUNG DES LYCOPIN-ZWISCHENPRODUKTS 3-甲基-4,4-二甲氧基-1-丁氧基

    公开(公告)号：EP2799418A1

    公开(公告)日：2014-11-05

    申请号：EP12862813.8

    申请日：2012-12-10

    申请人： Nanjing University Of Technology ,  Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory

    发明人： LV, Chunlei ,  PI, Shiqing ,  CHEN, Jianhui ,  LU, Dingqiang ,  OUYANG, Pingkai

    IPC分类号： C07C45/00 ,  C07C47/198

    CPC分类号： C07C45/30 ,  C07C41/22 ,  C07C45/00 ,  C07C45/516 ,  C07C47/198

    摘要： Disclosed is a preparation method of the lycopene intermediate 3-methyl-4,4-dialkoxy-1-butaldehyde. The preparation method comprises the following steps: (1) reacting 2-methyl-3,3-dialkoxy-1-halopropane with magnesium powder in the solvent of anhydrous tetrahydrofuran at a temperature of 45~65°C to generate a mixture of Grignard reagents under the protection of an inert gas; and (2) adding N,N-disubstituted carboxamide to the mixture of Grignard reagents and reacting at a temperature of 10°C~35°C to obtain 3-methyl-4,4-dialkoxy-1-butaldehyde. The process route of the present invention is simple and direct, the operation is easy, the conditions are mild and the yield is good, and thus the invention has commercial value.

    摘要翻译： 公开了番茄红素中间体3-甲基-4,4-二烷氧基-1-丁醛的制备方法。 制备方法包括以下步骤：（1）将4-甲基-3,3-二烷氧基-1-卤代丙烷与镁粉末在无水四氢呋喃的溶剂中在45〜65℃的温度下反应，生成格氏试剂 在惰性气体的保护下; 和（2）将N，N-二取代的甲酰胺加入到格氏试剂混合物中，并在10℃〜35℃的温度下反应，得到3-甲基-4,4-二烷氧基-1-丁醛。 本发明的工艺路线简单直接，操作容易，条件温和，产量好，因此本发明具有商业价值。

    PREPARATION METHOD OF 3,7,11-TRIMETHYLDODEC-2,4,6,10-TETRAENE-1-YL PHOSPHONIC SALT
    6.
    发明公开
    PREPARATION METHOD OF 3,7,11-TRIMETHYLDODEC-2,4,6,10-TETRAENE-1-YL PHOSPHONIC SALT 有权
    3,7,11-三甲基二烯-2,4,6,10-四萘-1-基膦酸盐的制备方法

    公开(公告)号：EP2799440A1

    公开(公告)日：2014-11-05

    申请号：EP12861708.1

    申请日：2012-12-10

    申请人： Nanjing University Of Technology ,  Zhejiang Medicine Co., Ltd. Xinchang Pharmaceutical Factory

    发明人： LV, Chunlei ,  PI, Shiqing ,  CHEN, Jianhui ,  LU, Dingqiang ,  OUYANG, Pingkai

    IPC分类号： C07F9/54

    CPC分类号： C07F9/5442 ,  C07F9/5428

    摘要： Provided in the present invention is a preparation method for a phosphonic salt, comprising the step of: reacting 3,7,11-trimethyldodec-1,4,6,10-tetraene-3-ol with triarylphosphine and an acid in an alcohol solvent at 50-100°C to form the phosphonic salt, wherein the acid is a sulfamic acid or methanesulfonic acid, and the alcohol solvent is a straight chain monohydric alcohol containing 1-5 carbon atoms. The method is performed in nearly neutral conditions, greatly reducing the generation of impurities and greatly obtaining phosphonic salt with an increased E content. The yield of lycopene obtained by using the phosphonic salt as a raw material is high.

    摘要翻译： 本发明提供了膦酸盐的制备方法，该方法包括以下步骤：使3,7,11-三甲基十二碳-1,4,6,10-四烯-3-醇与三芳基膦和酸在醇溶剂中反应 在50-100℃形成膦酸盐，其中酸是氨基磺酸或甲磺酸，醇溶剂是含1-5个碳原子的直链一元醇。 该方法在接近中性的条件下进行，大大减少了杂质的产生并大大地获得E含量增加的膦盐。 通过使用膦酸盐作为原料获得的番茄红素的产量很高。