Process for the preparation and isolation of 2-substituted tetrahydropyranols
    1.
    发明授权
    Process for the preparation and isolation of 2-substituted tetrahydropyranols 有权
    2-取代四氢吡喃醇的制备和分离方法

    公开(公告)号:US08791276B2

    公开(公告)日:2014-07-29

    申请号:US13157732

    申请日:2011-06-10

    IPC分类号: C07D309/10

    CPC分类号: C07D309/10

    摘要: Process for the preparation of 2-substituted 4-hydroxy-4-methyltetrahydropyrans of the formula (I) where the radical R1 is a straight-chain or branched alkyl or alkenyl radical having 1 to 12 carbon atoms, an optionally alkyl-substituted cycloalkyl radical having in total 3 to 12 carbon atoms or an optionally alkyl- and/or alkoxy-substituted aryl radical having in total 6 to 12 carbon atoms, comprising the reaction of 3-methylbut-3-en-1-ol of the formula (II) with an aldehyde of the formula (III) R1—CHO  (III), where the radical R1 has the same meaning as in formula (I) and where the reaction is carried out in the presence of water and in the presence of a strongly acidic cation exchanger, and then the isolation and/or the distillative separation is carried out in a dividing wall column or in an interconnection of (at least) two distillation columns in the form of a thermal coupling and one or more side take-off points at an absolute operating pressure of up to 500 mbar.

    摘要翻译: 用于制备式(I)的2-取代的4-羟基-4-甲基四氢吡喃的方法,其中基团R1是具有1至12个碳原子的直链或支链烷基或烯基,任选烷基取代的环烷基 具有总共3至12个碳原子的烷基和/或烷氧基取代的芳基,其总共包含6至12个碳原子,包括式(II)的3-甲基丁-3-烯-1-醇的反应 )与式(III)的醛R 1-CHO(III)反应,其中基团R 1具有与式(I)中相同的含义,并且其中反应在水的存在下并且在强烈存在下进行 酸性阳离子交换剂,然后分离和/或蒸馏分离在分隔壁塔中或在热耦合形式的(至少)两个蒸馏塔的互连中进行,并且一个或多个侧向起飞点 在绝对的工作压力高达500毫巴。

    Process for the Preparation and Isolation of 2-Substituted Tetrahydropyranols
    2.
    发明申请
    Process for the Preparation and Isolation of 2-Substituted Tetrahydropyranols 有权
    2-取代的四氢吡喃醇的制备和分离方法

    公开(公告)号:US20110306779A1

    公开(公告)日:2011-12-15

    申请号:US13157732

    申请日:2011-06-10

    IPC分类号: C07D309/10

    CPC分类号: C07D309/10

    摘要: Process for the preparation of 2-substituted 4-hydroxy-4-methyltetrahydropyrans of the formula (I) where the radical R1 is a straight-chain or branched alkyl or alkenyl radical having 1 to 12 carbon atoms, an optionally alkyl-substituted cycloalkyl radical having in total 3 to 12 carbon atoms or an optionally alkyl- and/or alkoxy-substituted aryl radical having in total 6 to 12 carbon atoms, comprising the reaction of 3-methylbut-3-en-1-ol of the formula (II) with an aldehyde of the formula (III) R1—CHO  (III), where the radical R1 has the same meaning as in formula (I) and where the reaction is carried out in the presence of water and in the presence of a strongly acidic cation exchanger, and then the isolation and/or the distillative separation is carried out in a dividing wall column or in an interconnection of (at least) two distillation columns in the form of a thermal coupling and one or more side take-off points at an absolute operating pressure of up to 500 mbar.

    摘要翻译: 用于制备式(I)的2-取代的4-羟基-4-甲基四氢吡喃的方法,其中基团R1是具有1至12个碳原子的直链或支链烷基或烯基,任选烷基取代的环烷基 具有总共3至12个碳原子的烷基和/或烷氧基取代的芳基,其总共包含6至12个碳原子,包括式(II)的3-甲基丁-3-烯-1-醇的反应 )与式(III)的醛R 1-CHO(III)反应,其中基团R 1具有与式(I)中相同的含义,并且其中反应在水的存在下并且在强烈存在下进行 酸性阳离子交换剂,然后分离和/或蒸馏分离在分隔壁塔中或在热耦合形式的(至少)两个蒸馏塔的互连中进行,并且一个或多个侧向起飞点 在绝对的工作压力高达500毫巴。

    METHOD FOR ISOLATING AMINES FROM AQUEOUS SOLUTIONS
    3.
    发明申请
    METHOD FOR ISOLATING AMINES FROM AQUEOUS SOLUTIONS 审中-公开
    从水溶液中分离氨的方法

    公开(公告)号:US20050000790A1

    公开(公告)日:2005-01-06

    申请号:US10494042

    申请日:2002-11-12

    CPC分类号: C07C209/86 C07C211/08

    摘要: A process for the isolation of amines from aqueous solutions by continuous distillation of aqueous solutions of the amines by a two-pressure method of rectifying aqueous solutions of amines which form with water an azeotrop, the composition of which is pressure-dependent, in two columns at different pressures provided that: a) the pressure in the second column is set to a value at least 0.5 bar higher than in the first column, b) the aqueous amine solution is fed, as a side stream, to the first column, and water and portions which boil at a higher temperature than the amine or which are non-volatile are removed at the base of the column, c) a mixture of amine and water is withdrawn at the head of the first column and fed, as a side stream, to the second column, d) an azeotrope of water and amine is withdrawn at the head of the second column and recycled to the first column, and (e) the purified amine is discharged at the base of the second column.

    摘要翻译: 一种通过连续蒸馏胺水溶液的方法,该方法是通过双向压力的方法将胺的水溶液与水形成,其组成为压力依赖性的两个塔 在不同的压力下,条件是:a)将第二塔中的压力设定为比第一塔高至少0.5巴的值,b)将胺水溶液作为侧流进料至第一塔,以及 在塔的底部除去水和在比不挥发性更高的温度下沸腾的部分,c)在第一塔的头部取出胺和水的混合物,并将其作为侧 流到第二塔,d)在第二塔的头部取出水和胺的共沸物并循环到第一塔,和(e)纯化的胺在第二塔的底部排出。

    Process for preparing M- or P-substituted phenylalkanols by alkylation
    4.
    发明授权
    Process for preparing M- or P-substituted phenylalkanols by alkylation 有权
    通过烷基化制备M-或P-取代的苯基链烷醇的方法

    公开(公告)号:US08692025B2

    公开(公告)日:2014-04-08

    申请号:US13503515

    申请日:2010-10-14

    IPC分类号: C07C45/29 C07C29/32

    摘要: The invention relates to a process for the preparation of m- or p-substituted phenylalkanols of the formula (I) in which R1 is bonded to the phenyl ring in the m- or p-position and is C1-C5-alkyl, and R2, R3, R4 and R5, independently of one another, are hydrogen or methyl, wherein an unsubstituted phenylalkanol of the formula (II) in which R2, R3, R4 and R5 have the meanings given under formula (I) is alkylated together with a C1-C5-alkyl halide of the formula (III) R1-Hal  (III), in which R1 has the meaning given under formula (I) and Hal is halogen, in the presence of a Friedel-Crafts catalyst to give an m- or p-alkyl-substituted phenylalkanol of the formula (I), then the reaction mixture is worked-up and the desired m- or p-alkyl-substituted phenylalkanol of the formula (I) is separated off, the other formed by-products are returned to the reaction mixture and these are isomerized in the presence of a Friedel-Crafts catalyst to give the desired m- or p-alkyl-substituted phenylalkanol. From the m- or p-alkyl-substituted phenylalkanols of the formula (I), it is possible to form, by oxidation or dehydrogenation, as products of value, the corresponding aldehydes, which play an interesting role as fragrances and aroma chemicals.

    摘要翻译: 本发明涉及一种制备式(I)的间 - 或对 - 取代的苯烷醇的方法,其中R 1与m-或p-位上的苯环键合并且是C1-C5-烷基,R2 R 3,R 4和R 5彼此独立地为氢或甲基,其中R 2,R 3,R 4和R 5具有式(I)所示含义的式(II)的未取代的苯基烷醇与 其中R 1具有式(I)所示含义,Hal为卤素的式(III)R1-Hal(Ⅲ)的C1-C5烷基卤化物,在Friedel-Crafts催化剂存在下,得到m- 或式(I)的对烷基取代的苯基链烷醇,然后将反应混合物处理并分离所需的式(I)的间 - 或对 - 烷基取代的苯基烷醇,另一个形成的副产物 返回到反应混合物中,并将它们在Friedel-Crafts催化剂存在下异构化,得到所需的间 - 或对 - 烷基取代的苯基 kanol 从式(I)的间 - 或对 - 烷基取代的苯烷醇,可以通过氧化或脱氢形成作为有价值的产物,相应的醛作为香料和香气化学品起着重要的作用。

    Fragrance Compositions Comprising Special Mixtures of Diastereomers of 2-Isobutyl-4-Methyl-Tetrahydro-2H-Pyran-4-OL
    5.
    发明申请
    Fragrance Compositions Comprising Special Mixtures of Diastereomers of 2-Isobutyl-4-Methyl-Tetrahydro-2H-Pyran-4-OL 审中-公开
    包含2-异丁基-4-甲基 - 四氢-2H-吡喃-4-醇的非对映异构体的特殊混合物的香料组合物

    公开(公告)号:US20130230476A1

    公开(公告)日:2013-09-05

    申请号:US13884503

    申请日:2011-11-08

    IPC分类号: C11B9/00

    CPC分类号: C11B9/008

    摘要: The present invention relates to a fragrance composition comprising a mixture of diastereomers of 2-isobutyl-4-methyl-tetrahydro-2H-pyran-4-ol, which comprises more than 95 wt. % of the optically inactive cis-racemate and less than 5 wt. % of the optically inactive trans-racemate. The present invention further relates to a method for producing a perfumed product or article as well as perfumed or aromatized articles comprising the fragrance compositions of the present invention.

    摘要翻译: 本发明涉及包含2-异丁基-4-甲基 - 四氢-2H-吡喃-4-醇的非对映异构体的混合物的香料组合物,其包含大于95wt。 %的光学活性的顺式外消旋物和小于5wt。 %的光学无活性反式外消旋物。 本发明还涉及一种用于生产加香产品或制品的方法,以及包含本发明的香料组合物的加香或芳香化制品。

    Preparation of 2-cyano-3,3-diarylacrylic esters
    6.
    发明授权
    Preparation of 2-cyano-3,3-diarylacrylic esters 失效
    制备2-氰基-3,3-二芳基丙烯酸酯

    公开(公告)号:US5917080A

    公开(公告)日:1999-06-29

    申请号:US952667

    申请日:1997-12-01

    CPC分类号: C07C253/30

    摘要: A process for preparing 2-cyano-3,3-diarylacrylic esters of the general formula I ##STR1## where R.sup.1 and R.sup.2 are hydrogen, C.sub.1 -C.sub.12 -alkyl groups, C.sub.- C.sub.12 -alkoxy groups or di(C.sub.1 -C.sub.4 -alkyl)amino groups and R.sup.3 is a C.sub.4 -C.sub.18 -alkyl group which can be interrupted by ether-functional oxygen atoms, by reacting a benzophenone imine of the general formula II ##STR2## with a cyanoacetic ester of the general formula III ##STR3## wherein the reaction is carried out at from 20 to 60.degree. C. and, during this, the liberated ammonia is continuously removed from the reaction mixture with the aid of a stream of gas or by reducing the pressure to from 900 to 100 mbar.

    摘要翻译: PCT No.PCT / EP96 / 02238 Sec。 371 1997年12月1日第 102(e)日期1997年12月1日PCT提交1996年5月24日PCT公布。 公开号WO96 / 38409 日期:1996年12月5日制备通式Ⅰ的2-氰基-3,3-二芳基丙烯酸酯的方法,其中R1和R2为氢,C1-C12-烷基,C-C12-烷氧基或二(C1-C4 - 烷基)氨基,R3是可以被醚官能的氧原子间隔的C4-C18-烷基,通过使通式II的二苯甲酮亚胺与通式III的氰基乙酸酯反应,其中反应进行 在20至60℃范围内,并且在此期间,借助于气流或通过将压力降低至900至100毫巴,将释放的氨从反应混合物中连续除去。

    Method for producing M-substituted phenylalkanols by means of isomerization
    8.
    发明授权
    Method for producing M-substituted phenylalkanols by means of isomerization 失效
    通过异构化制备M取代的苯基链烷醇的方法

    公开(公告)号:US08686193B2

    公开(公告)日:2014-04-01

    申请号:US13503488

    申请日:2010-10-19

    摘要: The invention relates to a process for the preparation of m-substituted phenylalkanols of the formula (I) in which R1 is C1-C5-alkyl and R2, R3, R4 and R5, independently of one another, are hydrogen or methyl, wherein a p-substituted phenylalkanol of the formula (II) in which R1, R2, R3, R4 and R5 having the meanings given under formula (I), is isomerized in the presence of a Friedel-Crafts catalyst to give an m-substituted phenylalkanol of the formula (I). From the m-substituted phenylalkanols of the formula (I) it is possible to form, by oxidation or dehydrogenation, as products of value, the corresponding aldehydes, which are known as fragrances and aroma chemicals.

    摘要翻译: 本发明涉及一种制备式(I)的间位取代的苯基烷醇的方法,其中R 1为C 1 -C 5 - 烷基且R 2,R 3,R 4和R 5彼此独立地为氢或甲基,其中a 式(II)的对取代的苯基链烷醇,其中具有式(I)给出的含义的R 1,R 2,R 3,R 4和R 5在Friedel-Crafts催化剂存在下异构化得到m-取代的苯基烷醇 式(I)。 从式(I)的间位取代的苯基烷醇可以通过氧化或脱氢形成作为有价值的产物,相应的醛被称为香料和芳香化学品。