Preparation of N-substituted pyrazoles
    1.
    发明授权
    Preparation of N-substituted pyrazoles 失效
    N-取代吡唑的制备

    公开(公告)号:US5468871A

    公开(公告)日:1995-11-21

    申请号:US334613

    申请日:1994-11-07

    摘要: N-substituted-pyrazoles of the formula ##STR1## wherein R.sup.1 is C.sub.1 -C.sub.12 -alkyl or C.sub.7 -C.sub.20 -alkyl, and R.sup.2, R.sup.3 and R.sup.4 independently denote hydrogen, C.sub.1 -C.sub.12 -alkyl, phenyl, C.sub.7 -C.sub.20 -alkylphenyl and C.sub.7 -C.sub.20 -phenylalkyl, are prepared by reacting a pyrazole of the formula ##STR2## wherein R.sup.2, R.sup.3 and R.sup.4 have the meanings above, with an alcohol or ether of the formulaR.sup.1 --O--R.sup.5 III,wherein R.sup.5 is hydrogen or R.sup.1, at a temperature of from 200.degree. to 550.degree. C. and a pressure of from 0.001 to 50 bar in the presence of a heterogeneous catalyst, preferably one which contains acid centers such as the oxides of aluminum, silicon, titanium and/or zirconium, optionally doped with phosphoric acid.

    摘要翻译: 其中R 1是C 1 -C 12 - 烷基或C 7 -C 20 - 烷基,R 2,R 3和R 4独立地表示氢,C 1 -C 12 - 烷基,苯基,C 7 -C 20 - 烷基苯基 和C 7 -C 20 - 苯基烷基,其通式如下:其中R2,R3和R4具有上述含义的吡唑与式R1-O-R5III的醇或醚反应制备,其中R 5是氢或 R1在200〜550℃的温度和0.001〜50巴的压力下,在非均相催化剂存在下,优选含有酸中心的铝,硅,钛和/或氧化物的氧化物 锆,任选掺杂有磷酸。

    Aqueous phase process for preparing N-substituted imidazoles
    2.
    发明授权
    Aqueous phase process for preparing N-substituted imidazoles 失效
    制备N-取代咪唑的水相方法

    公开(公告)号:US5877326A

    公开(公告)日:1999-03-02

    申请号:US914187

    申请日:1997-08-19

    摘要: A process for preparing substituted imidazoles of the formula I ##STR1## R.sup.1, R.sup.2 and R.sup.3 are identical or different and are each hydrogen, halogen, NO.sub.2, CN or a C.sub.1 -C.sub.20 -hydrocarbon radical which is unsubstituted or substituted by one or more halogens or R.sup.1 and R.sup.2 together are members of a 3- to 20-membered hydrocarbon ring which is unsubstituted or substituted by one or more halogens and/or C.sub.1 -C.sub.8 -alkyl groups and which may contain 1, 2 or 3 heteroatoms from the group consisting of nitrogen, oxygen and sulfur, andR.sup.4 is a C.sub.1 -C.sub.20 -hydrocarbon radical which is unsubstituted or substituted by one or more halogens,comprises using an aqueous phase of the imidazoles of the formula II ##STR2## where R.sup.1, R.sup.2 and R.sup.3 are as defined above with compounds of the formula IIIR.sup.4 --O--R.sup.5 IIIwhereR.sup.4 is as defined above andR.sup.5 is hydrogen or R.sup.4, it being possible in the latter case for the two R.sup.4 substituents to be identical or different,and reacting it at from 200.degree. to 550.degree. C. in the presence of a catalyst comprising oxides and/or phosphates of one or more metals of the 2nd, 3rd and 4th main group and the 4th subgroup of the Periodic Table in the presence or absence of phosphoric acid and/or phosphoric esters.

    摘要翻译: 制备式I的取代咪唑的方法R1,R2和R3相同或不同,各自为氢,卤素,NO2,CN或C1-C20-烃基,其未被取代或被一个或多个 卤素或R 1和R 2一起是3至20元烃环的成员,其未被取代或被一个或多个卤素和/或C 1 -C 8烷基取代,并且可以含有1,2或3个来自该基团的杂原子 由氮,氧和硫组成,R4是未被取代或被一个或多个卤素取代的C 1 -C 20烃基,包括使用式II的咪唑的水相,其中R 1,R 2和 R 3如上所定义,与式III的R4-O-R5III化合物,其中R 4如上定义,R 5是氢或R 4,在后一种情况下,两个R 4取代基可以相同或不同, 在约200℃〜550℃下, 在磷酸和/或磷酸酯存在或不存在的条件下,包含第2,第3和第4主族和第4族的周期表中的一种或多种金属的氧化物和/或磷酸盐。

    Preparation of ketones
    3.
    发明授权
    Preparation of ketones 失效
    酮的制备

    公开(公告)号:US4950763A

    公开(公告)日:1990-08-21

    申请号:US381469

    申请日:1989-07-18

    摘要: Ketones of the general formula (I) ##STR1## where R.sup.1 and R.sup.2 independently of one another are each alkyl, cycyloalkyl, arylalkyl, aryl or hetaryl, and one or more of the radicals R.sup.1 and R.sup.2 carry one or more hydrogen atoms on the .alpha.-carbon atom, are prepared by reacting two carboxylic acids of the general formulae (IIa/IIb), R.sup.1 --COOH (IIa) and R.sup.2 --COOH (IIb) or by reacting a carboxylic acid R.sup.1 --COOH (IIa) and a ketone ##STR2## or by reacting a mixture of IIa, IIb and Ib, in the gas phase in the presence of a catalyst, by a process in which a catalyst is used whose active material contains at least 50% by weight of titanium dioxide having a specific surface area greater than 10 m.sup.2 /g.0.

    摘要翻译: 其中R 1和R 2彼此独立地为烷基,氰基烷基,芳基烷基,芳基或杂芳基的通式(I)的酮,其中R 1和R 2中的一个或多个携带一个或多个氢原子 通过使通式(IIa / IIb),R1-COOH(IIa)和R2-COOH(IIb)的两种羧酸反应或通过使羧酸R1-COOH(IIa)和 酮(Ib)或IIa,IIb和Ib的混合物在气相中,在催化剂存在下,通过使用活性物质含有至少50重量%的催化剂的方法 的比表面积大于10m 2 / g的二氧化钛。

    Continuous preparation of alkyl esters of (meth)acrylic acid
    4.
    发明授权
    Continuous preparation of alkyl esters of (meth)acrylic acid 失效
    连续制备(甲基)丙烯酸的烷基酯

    公开(公告)号:US06072076A

    公开(公告)日:2000-06-06

    申请号:US789542

    申请日:1997-01-27

    CPC分类号: C07C67/08

    摘要: In a process for the continuous preparation of alkyl esters of (meth)acrylic acid by reacting (meth)acrylic acid with alkanols having from 1 to 8 carbon atoms in a homogeneous, liquid, solvent-free phase at elevated temperature and in the presence of an acid esterification catalyst, in which the (meth)acrylic acid, the alkanol and the acid catalyst are fed to a reaction zone, the water formed is removed by rectification during a residence time as constituent of a mixture comprising starting alkanol in a rectification unit (III) superposed on the reaction zone, the distillate obtained is separated into an organic phase comprising alkanol and an aqueous phase comprising water, the organic phase is essentially completely returned to the rectification unit (III), the reaction mixture is discharged from the reaction zone and conveyed into a distillative separation zone comprising further rectification units and in the latter the alkyl (meth)acrylate formed is separated off.a) (Meth)acrylic acid and alkanol are reacted in a molar ratio of from 1:0.75 to 1:2, b) part of the aqueous phase obtained at the top of the rectification unit (III) is returned to the rectification unit, c) the reaction mixture discharged from the reaction zone is fed to a further rectification unit (I) and in this the reaction mixture is separated into a product (II) comprising the catalyst and a product (I) comprising the alkyl ester of (meth)acrylic acid, remaining alkanol and remaining (meth)acrylic acid, and d) the product (I) is fed to a further rectification unit (II) and in this the alkyl ester of (meth)acrylic acid is separated from the remaining alkanol and from the remaining (meth)acrylic acid and the remaining alkanol and the remaining (meth)acrylic acid are returned to the reaction zone.

    摘要翻译: 在(甲基)丙烯酸的烷基酯的连续制备方法中,通过使(甲基)丙烯酸与具有1至8个碳原子的链烷醇在均相,液体,无溶剂相中在升高的温度下和在 将(甲基)丙烯酸,链烷醇和酸催化剂进料到反应区中的酸酯化催化剂,在停留时间内通过精馏除去形成的水,作为在精馏单元中起始烷醇的混合物的组分 (III),将获得的馏出物分离成包含链烷醇和含水的水相的有机相,有机相基本上完全返回到精馏单元(III),将反应混合物从反应物中排出 并输送到包含进一步精馏单元的蒸馏分离区中,后者分离形成的(甲基)丙烯酸烷基酯。 a)(甲基)丙烯酸和链烷醇的摩尔比为1:0.75至1:2,b)将在精馏单元(III)顶部获得的部分水相返回至精馏单元, c)将从反应区排出的反应混合物加入到另一精馏单元(I)中,并将反应混合物分离成包含催化剂的产物(II)和包含(甲基)丙烯酸烷基酯的产物(I) )丙烯酸,残留的链烷醇和剩余的(甲基)丙烯酸,以及d)将产物(I)加入到另一精馏单元(II)中,在此将(甲基)丙烯酸的烷基酯与剩余的链烷醇 和剩余的(甲基)丙烯酸和剩余的链烷醇和剩余的(甲基)丙烯酸返回到反应区。

    Preparation of acylated imidazoles
    6.
    发明授权
    Preparation of acylated imidazoles 失效
    酰化咪唑的制备

    公开(公告)号:US4924000A

    公开(公告)日:1990-05-08

    申请号:US321110

    申请日:1989-03-09

    CPC分类号: C07D233/64

    摘要: Acylated imidazoles of the formula ##STR1## where R.sup.1 and R.sup.3 are each H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, R.sup.4 is H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, and R.sup.5 is alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl, alkylaryl or carboxyl, are prepared by reacting imidazoles of the formula ##STR2## where R.sup.1, R.sup.2 and R.sup.3 are each alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, at least one of the radicals R.sup.1, R.sup.2 and R.sup.3 being hydrogen, and R.sup.4 is H, alkyl of from 1 to 12 carbon atoms, alkenyl of from 1 to 12 carbon atoms, aryl, aralkyl or alkylaryl, with widely used acylating agents of the formula ##STR3## where R.sup.5 is as defined above and Y is halide, alkoxy, acyloxy or hydroxyl, in the presence of acidic metal oxides and/or phosphates, preferably in the gas phase.

    摘要翻译: 其中R 1和R 3各自为H,具有1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,R 4为H,1至12的烷基, 碳原子,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,R5是1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基,烷基芳基或羧基, 使式(Ia)的咪唑与R1,R2和R3各自为1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,基团R1,R2和 R3为氢,R4为H,1至12个碳原子的烷基,1至12个碳原子的烯基,芳基,芳烷基或烷基芳基,以及广泛使用的通式为“IMAGE”的酰化剂,其中R5如上定义 在酸性金属氧化物和/或磷酸盐的存在下,优选在气相中,Y是卤化物,烷氧基,酰氧基或羟基。

    Preparation of 2-imidazolines
    9.
    发明授权
    Preparation of 2-imidazolines 失效
    2-咪唑啉的制备

    公开(公告)号:US4340745A

    公开(公告)日:1982-07-20

    申请号:US242011

    申请日:1981-03-09

    CPC分类号: C07D233/06

    摘要: 2-Imidazolines are prepared by reacting N,N'-diformyl-1,2-diamines in the gas phase at 200.degree.-350.degree. C., in the presence of certain amounts of an inert gas, over zinc oxide of a particular structure or over a mixture of this zinc oxide and aluminum oxide, as the catalyst.The 2-imidazolines obtainable by the process according to the invention are valuable starting materials for the preparation of dyes, crop protection agents and drugs.

    摘要翻译: 2-甲苯胺是通过使N,N'-二甲酰基-1,2-二胺在气相中在200-350℃下,在特定结构的氧化锌存在下,在一定量的惰性气体存在下, 或者该氧化锌和氧化铝的混合物,作为催化剂。 通过根据本发明的方法可获得的2-咪唑啉是制备染料,作物保护剂和药物的有价值的原料。

    Method for producing alkylene glycol with a low carbonyl compound content
    10.
    发明授权
    Method for producing alkylene glycol with a low carbonyl compound content 失效
    具有低羰基化合物含量的亚烷基二醇的制备方法

    公开(公告)号:US06329558B1

    公开(公告)日:2001-12-11

    申请号:US09581229

    申请日:2000-06-23

    IPC分类号: C07C2726

    摘要: In a process for isolating alkylene glycol having a low aldehyde content, in which a mixture comprising alkylene glycol is subjected to a final distillation, formic acid or a formate or a mixture of two or more formates or a mixture of formic acid and one or more formates is present in the mixture comprising alkylene glycol.

    摘要翻译: 在分离具有低醛含量的亚烷基二醇的方法中,其中使包含亚烷基二醇的混合物进行最终蒸馏,甲酸或甲酸盐或两种或更多种甲酸盐的混合物或甲酸和一种或多种 含有亚烷基二醇的混合物中存在甲酸盐。