Preparation of diamines
    32.
    发明授权
    Preparation of diamines 失效
    二胺的制备

    公开(公告)号:US5557011A

    公开(公告)日:1996-09-17

    申请号:US339916

    申请日:1994-11-15

    CPC分类号: C07C209/48

    摘要: Process for the preparation of diamines of the general formula I ##STR1## in which A denotes a C.sub.1 -C.sub.20 alkylene chain optionally mono- to penta-substituted by C.sub.1 -C.sub.4 alkyl,R.sup.1, R.sup.2 denote C.sub.1 -C.sub.20 alkyl, C.sub.1 -C.sub.20 hydroxyalkyl, C.sub.3 -C.sub.8 cycloalkyl, C.sub.4 -C.sub.20 alkylcycloalkyl, C.sub.4 -C.sub.20 cycloalkylalkyl, phenyl, C.sub.7 -C.sub.20 phenylalkyl, C.sub.1 -C.sub.20 alkoxyalkyl, C.sub.7 -C.sub.20 phenoxyalkyl or together a saturated or unsaturated C.sub.2 -C.sub.6 alkylene chain optionally monosubstituted, disubstituted, or trisubstituted by C.sub.1 -C.sub.4 alkyl and optionally interrupted by oxygen or nitrogen,by the reaction of dinitriles of the general formula IINC--A--CN (II),in which A has the aforementioned meaning,with secondary amines of the general formula II ##STR2## in which R.sup.1 and R.sup.2 have the aforementioned meanings, with hydrogen at temperatures ranging from 50.degree. to 200.degree. C. and pressures ranging from 5 to 300 bar in the presence of a hydrogenation catalyst, in which a palladium catalyst on an oxidic support is used as hydrogenation catalyst.

    摘要翻译: 制备通式I(II)的二胺的方法,其中A表示任选被C 1 -C 4烷基单取代至五取代的C 1 -C 20亚烷基链,R 1,R 2表示C 1 -C 20烷基,C 1 -C 20羟基烷基,C 3 -C 8环烷基,C 4 -C 20烷基环烷基,C 4 -C 20环烷基烷基,苯基,C 7 -C 20苯基烷基,C 1 -C 20烷氧基烷基,C 7 -C 20苯氧基烷基或一起饱和或不饱和的C 2 -C 6亚烷基链,任选单取代,二取代 或通过C 1 -C 4烷基三取代并且任选地被氧或氮中断,通过其中A具有上述含义的通式IINC-A-CN(II)的二腈与通式II的仲胺反应, 其中R 1和R 2具有上述含义,在氢化催化剂存在下,在氢气温度范围为50-200℃,压力范围为5-300巴,其中钯催化剂 在氧化载体上用作氢化催化剂 t。

    Decontamination of tertiary amines from primary and secondary amines
    33.
    发明授权
    Decontamination of tertiary amines from primary and secondary amines 失效
    从伯胺和仲胺去除叔胺

    公开(公告)号:US5481037A

    公开(公告)日:1996-01-02

    申请号:US299065

    申请日:1994-08-31

    CPC分类号: C07C209/84 C07C2101/14

    摘要: A process for the purification of tertiary amines in a crude mixture contaminated with undesirable primary and secondary amines which may have only a slight variance in boiling point with respect to the tertiary amine, wherein the crude mixture of the tertiary amine is treated at temperatures which may range from 0.degree. to 200.degree. C. but preferably from 20 to 150.degree. C. and at pressures of from 1 to 200 bar but most preferably under atmospheric pressure with a carboxylate of the formula ##STR1## in which R.sup.4 and R.sup.5 are selected from the group consisting of C.sub.1 -C.sub.20 -alkyl, C.sub.3 -C.sub.12 -cycloalkyl, C.sub.4 -C.sub.20 -cycloalkylalkyl, and aryl or C.sub.7 -C.sub.20 -aralkyl, both optionally mono- to penta- substituted by C.sub.1 -C.sub.8 -alkyl, C.sub.3 -C.sub.8 -cycloalkyl, or C.sub.4 -C.sub.12 -cycloalkylalkyl, and R.sup.4 may also represent hydrogen,to selectively form the alkylamides of the primary and secondary amine contaminants; and then separating the alkylamides from the tertiary amine by distillation.

    摘要翻译: 在不合适的伯胺和仲胺污染的粗混合物中纯化叔胺的方法,其可能在叔胺方面可能只有轻微的沸点变化,其中叔胺的粗混合物在 在0至200℃范围内,优选20至150℃,压力范围为1至200巴,最优选在大气压下,使用其中选择R 4和R 5的羧酸酯 由C 1 -C 20 - 烷基,C 3 -C 12 - 环烷基,C 4 -C 20 - 环烷基烷基和芳基或C 7 -C 20 - 芳烷基组成的组,任选被C 1 -C 8 - 烷基,C 3 -C 8 环烷基或C 4 -C 12环烷基烷基,并且R 4也可以代表氢,以选择性地形成伯胺和仲胺污染物的烷基酰胺; 然后通过蒸馏将烷基酰胺与叔胺分离。

    Process for the preparation of polyalcohols
    34.
    发明授权
    Process for the preparation of polyalcohols 失效
    制备多元醇的方法

    公开(公告)号:US6018074A

    公开(公告)日:2000-01-25

    申请号:US68300

    申请日:1998-10-05

    摘要: A process for the preparation of polyalcohols comprises the stages:(a) Reaction of an alkanal or ketone with formaldehyde in aqueous solution in the presence of a tertiary amine, to form a formates containing polyalcohol product mixture,(b) removal of water, excess tertiary amine, excess formaldehyde(c) heating of remaining mixture from (b) with removal of further formaldehyde and tertiary amine with formation of the formates of the polyalcohol,(d) transfer of tertiary amine removed from stage (b) and/or from stage (c), to synthesis stage (a) and/or to the subsequent transesterification stage (e),(e) transesterification of the resulting formates of the polyalcohol from stage (c) with an alcohol of the formula ROH in the presence of a transesterification catalyst to give polyalcohols and formates of the formula ##STR1## where R is a hydrocarbon radical, preferably alkyl of 1-6, particularly preferably 1-2, carbon atoms, and(f) isolation of the polyalcohols.

    摘要翻译: PCT No.PCT / EP96 / 04922 Sec。 371日期:1998年10月5日 102(e)日期1998年10月5日PCT 1996年11月11日PCT公布。 公开号WO97 / 17313 日期1997年5月15日制备多元醇的方法包括以下阶段:(a)在叔胺存在下,在水溶液中使烷醛或酮与甲醛反应,形成含有多元醇产物混合物的甲酸盐,(b) 的水,过量的叔胺,过量的甲醛(c)从(b)加热剩余的混合物,同时除去多元醇的甲酸盐形成的另外的甲醛和叔胺,(d)从阶段(b)中除去的叔胺的转移, 和(或)从阶段(c)到合成阶段(a)和/或后续酯交换反应阶段(e),(e)所得到的多元醇的甲酸酯从阶段(c)与式ROH的醇进行酯交换反应 在酯交换催化剂的存在下,得到下式的多元醇和甲酸盐,其中R是烃基,优选1-6的烷基,特别优选1-2的碳原子,和(f)多元醇的分离。

    Sterically hindered 4-amino-piperidine with a low dimer content, its
production and use
    35.
    发明授权
    Sterically hindered 4-amino-piperidine with a low dimer content, its production and use 失效
    四聚体含量低的4-氨基哌啶,其生产和使用

    公开(公告)号:US6013803A

    公开(公告)日:2000-01-11

    申请号:US180580

    申请日:1998-11-12

    CPC分类号: C08K5/3435 C07D211/58

    摘要: The invention relates to a process for reducing the dimerization of piperidines of the formula I ##STR1## where R.sup.1 to R.sup.4 are C.sub.1 - to C.sub.6 -alkyl, R.sup.1 and R.sup.2 and/or R.sup.3 and R.sup.4 together are a CH.sub.2 chain having 2 to 5 carbon atoms, which comprises adding to the piperidine from 0.001 to 0.2% by weight of a reducing agent of the formula MXH.sub.4-m Y.sub.m, where M is an alkali metal, NR.sub.4, where R are identical or different C.sub.1 -C.sub.4 -alkyl groups, or an equivalent of an alkaline earth metal or an equivalent of zinc, X is boron or aluminum, Y is H or CN and m is 0 or 1. The invention also relates to a mixture of piperidines of the formula I, from 0.001 to 0.2% by weight of a reducing agent and from 1 to 1000 ppm of dimers of the piperidines of the formula I, and to the preparation of hindered amine light stabilizers therefrom.

    摘要翻译: PCT No.PCT / EP97 / 02763 Sec。 371日期:1998年11月12日 102(e)1998年11月12日日期PCT提交1997年5月28日PCT公布。 出版物WO97 / 46528 日期1997年12月11日本发明涉及一种降低式Ⅰ哌啶的二聚的方法,其中R 1至R 4为C 1至C 6烷基,R 1和R 2和/或R 3和R 4一起为具有2至 5个碳原子,其包括向所述哌啶中添加0.001至0.2重量%的式MXH4-mYm的还原剂,其中M是碱金属,NR4,其中R是相同或不同的C 1 -C 4 - 烷基, 或当量的碱土金属或当量的锌,X为硼或铝,Y为H或CN,m为0或1.本发明还涉及式I的哌啶的混合物,为0.001至0.2 重量%的还原剂和1至1000ppm式I的哌啶的二聚体,以及由其制备受阻胺光稳定剂。

    Process for producing N-methyl-2(3,4 dimethoxyphenyl)-ethylamine
    36.
    发明授权
    Process for producing N-methyl-2(3,4 dimethoxyphenyl)-ethylamine 失效
    制备N-甲基-2(3,4-二甲氧基苯基) - 乙胺的方法

    公开(公告)号:US5840981A

    公开(公告)日:1998-11-24

    申请号:US945530

    申请日:1997-10-28

    摘要: A process for preparing N-methyl-2-(3,4-dimethoxyphenyl)-ethylamine comprises hydrogenating 3,4-dimethoxyphenylacetonitrile with a methylamine of the general formula I ##STR1## where R.sup.1 is hydrogen, benzyl or tert-butyl, and hydrogen in the presence of a supported catalyst which comprises from 0.05 to 50% by weight of copper chromite, copper, silver, gold, iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium, platinum or mixtures thereof, in the presence or absence of water at from 20.degree. to 200.degree. C. under from 1 to 300 bar.

    摘要翻译: PCT No.PCT / EP96 / 01861 Sec。 371日期1998年1月23日 102(e)日期1998年1月23日PCT提交1996年5月4日PCT公布。 公开号WO96 / 36589 日期:1996年11月21日制备N-甲基-2-(3,4-二甲氧基苯基) - 乙胺的方法包括用具有通式I的甲胺(I)氢化3,4-二甲氧基苯基乙腈,其中R1是氢, 苄基或叔丁基,和氢在负载催化剂存在下,其包含0.05至50重量%的亚铬酸铜,铜,银,金,铁,钴,镍,钌,铑,钯,锇,铱, 铂或其混合物,在存在或不存在20至200℃的水的条件下,在1至300巴下。

    Simultaneous preparation of caprolactam and hexamethylenediamine
    37.
    发明授权
    Simultaneous preparation of caprolactam and hexamethylenediamine 失效
    同时制备己内酰胺和己二胺

    公开(公告)号:US5717090A

    公开(公告)日:1998-02-10

    申请号:US565214

    申请日:1995-11-30

    IPC分类号: C07D201/08

    CPC分类号: C07D201/08

    摘要: Caprolactam and hexamethylenediamine are prepared simultaneously starting from adiponitrile by a process in which (a) adiponitrile is partially hydrogenated to give a mixture containing essentially 6-aminocapronitrile, hexamethylenediamine, ammonia, adiponitrile and hexamethyleneimine, (b) the mixture obtained in (a) is subjected to a distillation to give ammonia as the top product and a bottom product I, (c) the bottom product I containing essentially 6-aminocapronitrile, hexamethylenediamine, adiponitrile, hexamethyleneimine, inert compound A and ammonia, the ammonia content being lower than that of the mixture used in stage (b), is subjected to a second distillation to give a mixture comprising the inert compound A and ammonia as the top product and a bottom product II, (d) the bottom product II is subjected, in a third column, to a distillation to give the inert compound A as the top product and a bottom product III, (e) the bottom product III is subjected, in a fourth column, to a distillation to give a top product KP1, containing essentially hexamethyleneimine and a bottom product IV, (f) the top product KP1 is subjected, in a fifth column, to a distillation to give a top product KP2, which contains essentially hexamethyleneimine, and (g) the bottom product IV containing essentially 6-aminocapronitrile and adiponitrile is subjected, in a sixth column, to a distillation to give 6-aminocapronitrile, and the 6-aminocapronitrile thus obtained is then cyclized to give caprolactam.

    摘要翻译: 己二醇和六亚甲基二胺由己二腈通过以下方法同时制备,其中(a)己二腈部分氢化得到基本上含有6-氨基己腈,六亚甲基二胺,氨,己二腈和六亚甲基亚胺的混合物,(b)将(a)中得到的混合物 进行蒸馏以产生氨作为顶部产物,底部产物I,(c)含有基本上为6-氨基己腈,六亚甲基二胺,己二腈,六亚甲基亚胺,惰性化合物A和氨的底部产物I,氨含量低于 将阶段(b)中使用的混合物进行第二次蒸馏,得到包含惰性化合物A和氨作为顶部产物的混合物和底部产物II,(d)底部产物II经受第三塔 进行蒸馏,得到惰性化合物A作为顶部产物和底部产物III,(e)底部产物III在第四列中经受 蒸馏得到基本上为六亚甲基亚胺和底部产物IV的顶部产物KP1,(f)顶部产物KP1在第五个塔中进行蒸馏,得到基本上含有六亚甲基亚胺的顶部产物KP2,和(g )将含有基本上6-氨基己腈和己二腈的底部产物IV在第六塔中进行蒸馏以得到6-氨基己腈,然后将所得的6-氨基己腈环化,得到己内酰胺。

    Preparation of aliphatic alpha, omega-aminonitriles
    39.
    发明授权
    Preparation of aliphatic alpha, omega-aminonitriles 失效
    脂肪族α,ω-氨基腈的制备

    公开(公告)号:US5527946A

    公开(公告)日:1996-06-18

    申请号:US375573

    申请日:1995-01-18

    摘要: Aliphatic alpha, omega-aminonitriles are prepared by partial hydrogenation of aliphatic alpha, omega-dinitriles at elevated temperatures and superatmospheric pressure in the presence of a solvent and of a catalyst by a process which comprises using a catalyst which(a) contains a compound based on a metal selected from the group consisting of nickel, cobalt, iron, ruthenium and rhodium and(b) contains from 0.01 to 25% by weight, based on (a), of a promoter based on a metal selected from the group consisting of palladium, platinum, iridium, osmium, copper, silver, gold, chromium, molybdenum, tungsten, manganese, rhenium, zinc, cadmium, lead, aluminum, tin, phosphorus, arsenic, antimony, bismuth and rare earth metals and(c) from 0 to 5% by weight, based on (a), of a compound based on an alkali metal or on an alkaline earth metal,with the proviso that the component (a) is not based on iron or iron and one of the metals selected from the group consisting of cobalt, ruthenium and rhodium when (b) is a promoter based on a metal selected from the group consisting of titanium, manganese, chromium and molybdenum, and with the further proviso that, when a compound based on only ruthenium or rhodium or ruthenium and rhodium or nickel and rhodium is selected as component (a), the promoter (b) may be dispensed with.

    摘要翻译: 脂肪族α,ω-氨基腈通过脂肪族α,ω-二腈在升高的温度和超大气压下,在溶剂和催化剂存在下通过包括使用(a)含有基于化合物的催化剂 在选自镍,钴,铁,钌和铑的金属上,和(b)含有基于(a)0.01至25重量%的基于选自以下的金属的促进剂: 钯,铂,铱,锇,铜,银,金,铬,钼,钨,锰,铼,锌,镉,铅,铝,锡,磷,砷,锑,铋和稀土金属和(c) 基于(a),基于碱金属或碱土金属的化合物为0至5重量%,条件是组分(a)不以铁或铁为基准,并且所选择的金属之一 由钴,钌和铑组成 当(b)是基于选自钛,锰,铬和钼的金属的促进剂时,另外条件是当仅基于钌或铑或钌和铑或镍和铑的化合物为 作为组分(a)选择,可以不用启动子(b)。