Preparation of 2-(3-aminopropyl)-cycloalkylamines
    1.
    发明授权
    Preparation of 2-(3-aminopropyl)-cycloalkylamines 失效
    2-(3-氨基丙基) - 环丙基胺的制备

    公开(公告)号:US5239120A

    公开(公告)日:1993-08-24

    申请号:US676087

    申请日:1991-03-27

    摘要: A process for the preparation of a 2-(3-aminopropyl)-cycloalkylamine of the general formula I ##STR1## in which the subscript n is an integer from 1 to 4, from a 2-(2-cyanoethyl)-cycloalkanone of the general formula II ##STR2## in which the subscript n has the meaning stated, wherein the following stages are carried out in discrete reaction chambers:a) the 2-(2-cyanoethyl)-cycloalkanone of formula II is reacted in a first reaction chamber with excess ammonia over an acidic heterogeneous catalyst at a temperature from 20.degree. to 150.degree. C. and a pressure of from 15 to 500 bar, andb) in a second reaction chamber, the reaction product from stage a) is hydrogenated at a temperature of from 60.degree. to 150.degree. C. and a pressure of from 50 to 300 bar in the presence of excess ammonia over a catalyst containing cobalt, nickel, ruthenium, and/or some other noble metal, which catalyst optionally contains a basic component or is supported on neutral or basic supporting material.

    摘要翻译: 2-(2-氰基乙基) - (2-氨基丙基) - 环烷基胺的制备方法,其中下标n为1至4的整数,通式I(I) 通式II(II)的环烷酮,其中下标n具有所述的含义,其中以下步骤在离散的反应室中进行:a)式II的2-(2-氰基乙基) - 环烷酮是 在酸性多相催化剂的第一反应室中,在第二反应室中,在20至150℃的温度和15至500巴的压力下,在第一反应室中与过量的氨反应,和b)在第二反应室中,反应产物从步骤a )在过量氨的存在下在含有钴,镍,钌和/或一些其它贵金属的催化剂的温度下在60至150℃的温度和50至300巴的压力下氢化,该催化剂 可选地含有基本组分或者在中性或基础支撑材料上支撑。

    Preparation of 3-aminomethyl-3,5,5-trimethyl-cyclohexylamine
    2.
    发明授权
    Preparation of 3-aminomethyl-3,5,5-trimethyl-cyclohexylamine 失效
    3-氨基甲基-3,5,5-三甲基 - 环己胺的制备

    公开(公告)号:US5371292A

    公开(公告)日:1994-12-06

    申请号:US92029

    申请日:1993-07-15

    摘要: A process for the preparation of 3-aminomethyl-3,5,5-trimethyl-cyclohexylamine from 3-cyano-3,5,5-trimethyl-cyclohexanone, wherein the following stages are carried out in discrete reaction chambers:a) the 3-cyano-3,5,5-trimethyl-cyclohexanone is reacted in a first reaction chamber with excess ammonia over an acidic metal oxide catalyst at a temperature of from 20.degree. to 150.degree. C. and a pressure of from 15 to 500 bar, andb) in a second reaction chamber, the reaction product from stage a) is hydrogenated with hydrogen at a temperature of from 60.degree. to 150.degree. C. and a pressure of from 50 to 300 bar in the presence of excess ammonia over a catalyst containing cobalt, nickel, ruthenium, and/or some other noble metal, which catalyst optionally contains a basic component or is supported by neutral or basic supporting material.

    摘要翻译: 从3-氰基-3,5,5-三甲基 - 环己酮制备3-氨基甲基-3,5,5-三甲基 - 环己胺的方法,其中以下步骤在离散反应室中进行:a)3 氰基-3,5,5-三甲基 - 环己酮在第一反应室中与过量的氨在酸性金属氧化物催化剂上在20至150℃的温度和15至500巴的压力下反应, 和b)在第二反应室中,在过量的氨在催化剂存在下,将氢气从60℃升至150℃,压力为50-300巴,在步骤a)中的反应产物被氢化 含有钴,镍,钌和/或一些其它贵金属,该催化剂任选地含有碱性组分或由中性或碱性载体材料负载。

    Preparation of 2,2-disubstituted pentane-1,5-diamines
    3.
    发明授权
    Preparation of 2,2-disubstituted pentane-1,5-diamines 失效
    2,2-取代的戊烷-1,5-二胺的制备

    公开(公告)号:US5166443A

    公开(公告)日:1992-11-24

    申请号:US676086

    申请日:1991-03-17

    CPC分类号: C07C209/48 C07C211/09

    摘要: A process for the preparation of a 2,2-disubstituted pentane-1,5-diamine of the formula I ##STR1## where R.sup.1 and R.sup.2, independently of one another, are C.sub.1 - to C.sub.10 -alkyl or C.sub.2 - to C.sub.10 -alkenyl or together are a C.sub.4 - to C.sub.7 -alkylene chain which is unsubstituted or monosubstituted to pentasubstituted by C.sub.1 - to C.sub.4 -alkyl, from a 2,2-disubstituted 4-cyanobutanal of the formula II ##STR2## where R.sup.1 and R.sup.2 are as defined above, comprises, in two spatially separate reaction spaces,a) reacting the 4-cyanobutanal of the formula II, in a first reaction space, with excess ammonia on an acidic heterogeneous catalyst at from 20.degree. to 150.degree. C. and at from 15 to 500 bar, andb) hydrogenating the resultant reaction product, in a second reaction space, using excess hydrogen in the presence of excess ammonia on a catalyst containing cobalt, nickel, ruthenium and/or another noble metal, if desired with a basic component or on a basic or neutral carrier, at from 60.degree. to 150.degree. C. and at from 50 to 500 bar.

    摘要翻译: 制备式I(I)的2,2-二取代戊烷-1,5-二胺的方法,其中R 1和R 2彼此独立地为C 1至C 10烷基或C 2至 C10链烯基或一起是未被取代或被C1至C4-烷基单取代至五取代的C 4 -C 7亚烷基链,其由式II(II)的2,2-二取代4-氰基丁醛代替,其中 R1和R2如上定义,在两个空间上分开的反应空间中包含a)在第一反应空间中使式II的4-氰基丁醛与过量的氨在20-150℃的酸性多相催化剂上反应 和b)在第二反应空间中,在过量的氨存在下,使用过量的氢在含有钴,镍,钌和/或其它贵金属的催化剂上氢化所得反应产物, 如果需要,可以使用碱性组分或碱性或中性载体,在60至150℃和50至50℃ 500吧。

    Selective preparation of linear pentane-1,5-diamines in increased yields
    5.
    发明授权
    Selective preparation of linear pentane-1,5-diamines in increased yields 失效
    线性戊烷-1,5-二胺的选择性制备

    公开(公告)号:US5344983A

    公开(公告)日:1994-09-06

    申请号:US936084

    申请日:1992-08-26

    CPC分类号: C07C209/48

    摘要: Process for preparing a pentane-1,5-diamine of the formula ##STR1## where R.sup.1 represents a variety of organic radicals including alkyl which can bear substituents such as hydroxyl, halogen, alkoxy, carbalkoxy, carboxyl, alkylamino, cycloalkyl or aryl, andR.sup.2 and R.sup.3 independently of one another, represent hydrogen or have the same meanings as R.sup.1 or together are a C.sub.4 -C.sub.7 -alkylene chain which is unsubstituted or substituted by one to five C.sub.1 -C.sub.4 -alkyl groups,which comprises:(a) reacting a .gamma.-cyanoketone of the formula ##STR2## where R.sup.1, R.sup.2 and R.sup.3 have the meanings given above, with excess ammonia in a first reaction space on an acidic heterogeneous catalyst at 20.degree.-150.degree. C. and 15-500 bar, and(b) hydrogenating the resulting reaction product in a second separate reaction space in the presence of excess ammonia on a cobalt, nickel or noble metal catalyst at 50.degree.-180.degree. C. and 30-500 bar.Novel pentane-1,5-diamines are obtained, in which R.sup.1 must contain at least two carbon atoms if R.sup.2 and R.sup.3 are both hydrogen. These new compounds containing two primary amine groups possess advantageous properties of lower volatility and also greater asymmetry (with different reactivity of the two amine functions). They provide useful curing agents for epoxides and act as improved components of polyamides.

    摘要翻译: 制备式(I)的戊烷-1,5-二胺的方法,其中R 1表示各种有机基团,包括可以带有取代基的烷基,例如羟基,卤素,烷氧基,烷氧基,羧基,烷基氨基,环烷基或 芳基和R 2和R 3彼此独立地表示氢或具有与R 1相同的含义或一起是未被取代或被一至五个C 1 -C 4 - 烷基取代的C 4 -C 7亚烷基链,其包含:( a)在20-150℃的酸性非均相催化剂的第一反应空间中使具有上述含义的式(Ia)的式(II)的γ-氰基酮与过量的氨反应,其中R1,R2和R3具有上述含义, 15-500巴,(b)在钴,镍或贵金属催化剂的存在下,在50-180℃和30-500巴下,在第二分开的反应空间中,使得到的反应产物氢化。 得到新的戊烷-1,5-二胺,如果R2和R3都是氢,其中R1必须含有至少两个碳原子。 这些含有两个伯胺基团的新化合物具有较低的挥发性和更大的不对称性(两种胺官能团的不同反应性)的有利特性。 它们为环氧化物提供有用的固化剂,并且作为聚酰胺的改进组分。

    Joint preparation of 3-dialkylaminopropionitriles, bis-(2-cyanoethyl)
ether and, if desired, ethylene-cyanohydrin
    9.
    发明授权
    Joint preparation of 3-dialkylaminopropionitriles, bis-(2-cyanoethyl) ether and, if desired, ethylene-cyanohydrin 失效
    联合制备3-二烷基氨基丙腈,双(2-氰基乙基)醚和(如果需要)乙烯 - 氰醇

    公开(公告)号:US4965362A

    公开(公告)日:1990-10-23

    申请号:US376373

    申请日:1989-07-06

    摘要: 3-Dialkylaminopropionitriles ##STR1## where R.sup.1 and R.sup.2 are each C.sub.1 -C.sub.4 -alkyl which may furthermore be bonded to form a 5-membered or 6-membered ring, bis-(2-cyanoethyl) ether IINC--CH.sub.2 --CH.sub.2 --O--CH.sub.2 --CH.sub.2 --CN IIand, if desired, ethylenecyanohydrin IIIHO--CH.sub.2 --CH.sub.2 --CN IIIare prepared jointly by a process in which(a) acrylonitrile and water are reacted in the presence of a base at from 60.degree. to 150.degree. C. to give a mixture of acrylonitrile, water and bis-(2-cyanoethyl) ether II, the base being a mineral base, a quaternary nitrogen base or a mixture of these,(b) this mixture is reacted at about 0.degree.-50.degree. C. with a dialkylamine of the general formula IV ##STR2## to give a mixture of water, a dialkylaminopropionitrile I and bis-(2-cyanoethyl) ether II, and this mixture is separated into its components and(c) if desired, the ether II obtained in proces stage (b) or an aqueous solution of this ether and/or the reacted mixtures containing this ether and obtained from process stage (a) or (b) is allowed to react at from 50.degree. to 150.degree. C. with the dialkylamine IV to give a mixture of a 3-dialkylaminopropionitrile I and ethylenecyanohydrin III, and, if desired, the said mixture is separated into its components.

    摘要翻译: 3-二烷基氨基丙腈其中R 1和R 2各自为可以连接形成5元或6元环的C 1 -C 4 - 烷基,双 - (2-氰基乙基)醚II NC-CH 2 -CH 2 - O-CH 2 -CH 2 -CN II和如果需要,乙烯基氰醇III HO-CH 2 -CH 2 -CN III通过以下方法共同制备,其中(a)丙烯腈和水在碱的存在下在60℃至 150℃,得到丙烯腈,水和双 - (2-氰基乙基)醚II的混合物,碱为矿物碱,季氮碱或它们的混合物,(b)该混合物在约0℃ 与二烷基胺(通式IV IV)反应,得到水,二烷基氨基丙腈I和双 - (2-氰基乙基)醚II的混合物,将该混合物分离成其组分,(c )如果需要,在步骤阶段(b)中获得的醚II或该醚的水溶液和/或含有该醚的反应混合物从工艺步骤(a)或(b)获得, 使其与二烷基胺IV在50-150℃下反应,得到3-二烷基氨基丙腈I和乙基烯丙醇III的混合物,如果需要,将所述混合物分离成其组分。

    Preparation of caprolactam
    10.
    发明授权
    Preparation of caprolactam 失效
    己内酰胺的制备

    公开(公告)号:US4963672A

    公开(公告)日:1990-10-16

    申请号:US448899

    申请日:1989-12-12

    CPC分类号: C07D201/08 Y02P20/52

    摘要: Caprolactam is prepared in a process comprising the following steps:(a) reacting the 5-formylvaleric ester with liquid ammonia as reaction medium and hydrogen in the presence of a ruthenium catalyst in liquid phase at from 80.degree. to 140.degree. C. under a hydrogen partial pressure of from 40 to 100 bar,(b) replacing the reaction medium ammonia by an aromatic hydrocarbon having a boiling point of from 80.degree. to 240.degree. C. which is liquid under the reaction conditions,(c) heating the resulting mixture in liquid phase under superatmospheric pressure at 230.degree.-350.degree. C. to form caprolactam, and(d) isolating caprolactam from the resulting reaction mixture.

    摘要翻译: 己内酰胺以包括以下步骤的方法制备:(a)使5-甲酰基戊酸酯与液氨作为反应介质和氢在钌催化剂存在下在液相中在80-140℃下在氢气 分压为40〜100巴,(b)在反应条件下用沸点为80〜240℃的芳烃替代反应介质氨,(c)将所得混合物加热 液相在超大气压下在230-350℃下反应形成己内酰胺,和(d)从所得反应混合物中分离己内酰胺。