Preparation of 5-methylbutyrolactone
    4.
    发明授权
    Preparation of 5-methylbutyrolactone 失效
    5-甲基丁酰胺的制备

    公开(公告)号:US5189182A

    公开(公告)日:1993-02-23

    申请号:US236199

    申请日:1988-08-25

    IPC分类号: C07D315/00

    CPC分类号: C07D315/00

    摘要: 5-Methylbutyrolactone is prepared by a process in which a pentenoic ester of the formula IX--CO.sub.2 R (I),where X is CH.sub.2 .dbd.CH--CH.sub.2 --CH.sub.2 --, CH.sub.3 --CH.dbd.CH--CH.sub.2 -- or CH.sub.3 --CH.sub.2 --CH.dbd.CH-- and R is alkyl, cycloalkyl, aralkyl or aryl, or a mixture of these esters is reacted with water at from 50.degree. to 350.degree. C. in the presence or absence of a diluenta) over a zeolite and/or phosphate catalyst orb) in the presence of from 0.01 to 0.25 mole of a sulfonic acid, a Lewis acid and/or a non-oxidizing mineral acid per mole of pentenoic ester or over from 0.1 to 40% by weight, based on the pentenoic ester, of a strongly acidic ion exchanger as a catalyst in a first stage, or the pentenoic ester of the formula I, where X and R have the stated meanings, is hydrolyzed in a first stage with the aid of a strongly acidic ion exchanger as a catalyst to give the pentenoic acid of the formula I, where R is hydrogen, and the resulting pentenoic acid is subjected to cyclization in a second stage in the presence of from 0.005 to 0.1 mole of a sulfonic acid, a Lewis acid or a non-oxidizing mineral acid per mole of pentenoic acid or over from 0.1 to 20% by weight, based on the pentenoic acid, of a strongly acidic ion exchanger at from 50.degree. to 350.degree. C.

    摘要翻译: 通过以下方法制备5-甲基丁内酯,其中式I X-CO 2 R(I)的戊烯酸酯,其中X为CH 2 = CH-CH 2 -CH 2 - ,CH 3 -CH = CH-CH 2 - 或CH 3 -CH 2 -CH = CH-和R是烷基,环烷基,芳烷基或芳基,或这些酯的混合物与水在50-350℃下在存在或不存在稀释剂a)的情况下与沸石和/或磷酸盐 催化剂或b)在0.01至0.25摩尔磺酸,路易斯酸和/或非氧化性无机酸/摩尔烯酸酯存在下或基于戊烯酸酯为0.1至40重量% 的作为第一阶段的催化剂的强酸性离子交换剂或其中X和R具有所述含义的式I的戊烯酸在第一阶段中借助于强酸性离子交换剂作为 催化剂得到式I的戊烯酸,其中R是氢,所得戊烯酸在第二阶段中在0.005t的存在下进行环化 o 0.1摩尔磺酸,路易斯酸或非氧化性无机酸/摩尔烯酸,或超过0.1-20重量%,基于戊烯酸,强酸性离子交换剂为50〜 350℃

    Preparation of 5-formylvaleric esters
    5.
    发明授权
    Preparation of 5-formylvaleric esters 失效
    5-甲酰戊酸酯的制备

    公开(公告)号:US5003102A

    公开(公告)日:1991-03-26

    申请号:US206751

    申请日:1988-06-15

    CPC分类号: C07C67/347

    摘要: 5-Formylvaleric esters are prepared by a process which comprises the following steps:(a) Hydroformylation of a pentenoic ester by reaction with carbon monoxide and hydrogen at elevated temperatures and under superatmospheric pressure in the presence of a carbonyl complex of a metal of group 8 of the Periodic Table with formation of a mixture of 5-, 4- and 3-formylvaleric esters,(b) Isolation of the 5-formylvaleric ester from the resulting mixture of 5-, 4- and 3-formylvaleric esters, a mixture essentially consisting of 4- and 3-formylvaleric esters remaining,(c) Cleavage of the mixture essentially consisting of 4- and 3-formylvaleric esters at from 50.degree. to 400.degree. C. in the presence of a catalyst to give pentenoic esters and(d) Recycling of the pentenoic esters to stage (a).

    摘要翻译: 5-甲酰戊酸酯通过包括以下步骤的方法制备:(a)在升高的温度和超大气压下,在第8组的金属的羰基络合物存在下,通过与一氧化碳和氢气反应来进行戊烯基酯的加氢甲酰化 的化合物,形成5-,4-和3-甲酰基戊酸酯的混合物,(b)从得到的5-,4-和3-甲酰基戊酸酯混合物中分离5-甲酰基戊酸酯,基本上 由4-和3-甲酰基戊酸酯组成,(c)在催化剂存在下,在50-400℃下将基本上由4-和3-甲酰基戊酸酯组成的混合物切割,得到戊烯酸酯和(d )将戊烯酸酯循环回到(a)阶段。

    Process for the preparation of a hydrogenation catalyst
    7.
    发明授权
    Process for the preparation of a hydrogenation catalyst 失效
    制备氢化催化剂的方法

    公开(公告)号:US5817592A

    公开(公告)日:1998-10-06

    申请号:US590455

    申请日:1996-01-23

    摘要: A process for the preparation of a hydrogenation catalyst by reduction of platinum in an oxidation stage of not less than 2 in an aqueous medium in the presence of a carboniferous support, optionally following partial poisoning with a sulfur, arsenic, tellurium, or antimony-containing compound, using a reducing agent, in which the reducing agent used is an ammonium or phosphonium salt of the general formula I �XR.sup.4 !.sub.n Y I in which X stands for N or P, R stands for hydrogen, C.sub.1 --C.sub.18 alkyl, C.sub.5 --C.sub.10 cycloalkyl, phenyl radical, and also a C.sub.1 --C.sub.4 alkyl radical substituted by phenyl, the phenyl radicals being mono-to tri-substituted by C.sub.1 --C.sub.6 alkyl, halogen, nitro or amino, if desired, provided that the radicals R may be the same or different but cannot simultaneously denote hydrogen, if X is P, n is an integer of 1 to 3, and Y is an organic anion which can reduce platinum in an oxidation stage other than zero to platinum in the oxidation stage of zero.

    摘要翻译: 一种通过在含水载体的存在下在水性介质中在不少于2的氧化阶段还原铂的氢化催化剂的方法,任选地在用硫,砷,碲或含锑的部分中毒后 化合物,使用还原剂,其中所用的还原剂是通式I [XR4] nYinin的铵盐或鏻盐,其中X代表N或P,R代表氢,C1-C18烷基,C5-C10环烷基 苯基,以及被苯基取代的C1-C4烷基,如果需要,苯基由C1-C6烷基,卤素,硝基或氨基单取代至三取代,条件是基团R可以相同 或不同,但不能同时表示氢,如果X为P,n为1至3的整数,Y为有机阴离子,在氧化阶段为零的情况下,铂可以在除氧以外的氧化阶段中还原为铂。

    Manufacture of pent-3-enoic acid and its alkyl esters
    9.
    发明授权
    Manufacture of pent-3-enoic acid and its alkyl esters 失效
    戊-3-烯酸及其烷基酯的制备

    公开(公告)号:US4550195A

    公开(公告)日:1985-10-29

    申请号:US295088

    申请日:1981-08-21

    CPC分类号: C07C51/14

    摘要: A process for the manufacture of pent-3-enoic acid and its alkyl esters, of the general formulaCH.sub.3 --CH.dbd.CH--CH.sub.2 --CO--ORwhere R is hydrogen or alkyl of 1 to 4 carbon atoms, comprising carbonylating butadiene with carbon monoxide and a compound ROH at from 300 to 1,000 bars CO pressure and from 100.degree. to 160.degree. C. in the presence of cobalt catalysts and nitrogen bases, wherein C.sub.4 cuts are used as starting materials and a tertiary amine having a pK.sub.A of from 3 to 11 is used as the nitrogen base. The pent-3-enoic acid or alkyl esters produced may be used for the manufacture of adipic acid or its alkyl esters, which compounds are starting materials for the manufacture of nylons.

    摘要翻译: 制备通式为CH 3 -CH = CH-CH 2 -CO-OR的戊-3-烯酸及其烷基酯的方法,其中R是氢或1至4个碳原子的烷基,其包括将碳酸丁二烯与碳 在钴催化剂和氮碱的存在下,在300至1,000巴CO压力和100至160℃下进行一氧化碳和化合物ROH,其中使用C4馏分作为起始原料,并使用pKA为3的叔胺 至11为氮基。 所制备的戊-3-烯酸或烷基酯可用于制造己二酸或其烷基酯,该化合物是用于制造尼龙的起始原料。

    Preparation of butanedicarboxylic esters
    10.
    发明授权
    Preparation of butanedicarboxylic esters 失效
    丁烷二羧酸酯的制备

    公开(公告)号:US4310686A

    公开(公告)日:1982-01-12

    申请号:US153572

    申请日:1980-05-27

    CPC分类号: C07C69/34 C07C67/38

    摘要: A process for the preparation of butanedicarboxylic acid esters, wherein(a) an aqueous cobalt salt solution is treated with excess carbon monoxide and hydrogen in the presence of active charcoal laden with cobalt carbonyl,(b) the resulting aqueous solution of cobalt carbonyl hydride is extracted with butadiene or a butadiene containing hydrocarbon mixture and the aqueous phase is separated off,(c) the butadiene, or butadiene/hydrocarbon mixture, containing cobalt carbonyl hydride, cobalt carbonyl and butenyl-cobalt tricarbonyl, is reacted with carbon monoxide and excess C.sub.1 -C.sub.4 -alkanol in the presence of a tertiary nitrogen base,(d) the resulting reaction mixture is freed from the tertiary nitrogen base contained therein, down to a content of from 0.1 to 0.3 mole per mole of pentenoic acid ester, and from excess hydrocarbons, and the pentenoic acid ester remaining in the reaction mixture is reacted with carbon monoxide and excess C.sub.1 -C.sub.4 -alkanol in the presence of the cobalt carbonyl and tertiary nitrogen base contained in the reaction mixture,(e) the reaction mixture is treated with an oxidizing agent in the presence of the aqueous acid solution which has been separated off in stage (b), and the mixture is separated into an organic phase, from which butanedicarboxylic acid esters are isolated by distillation, and an aqueous phase, and(f) the aqueous phase is extracted with water-immiscible solvents, the phases are separated, and the resulting aqueous phase is freed from alkanols and tertiary nitrogen base and is recycled to stage (a).

    摘要翻译: 制备丁烷二羧酸酯的方法,其中(a)钴水溶液在过量的一氧化碳和氢气的存在下,在负载有羰基钴的活性炭存在下处理,(b)得到的氢化羰基碳水溶液为 用丁二烯或含丁二烯的烃混合物萃取并分离出水相,(c)含有羰基氢化钴,羰基钴和三丁基钴的三羰基化合物的丁二烯或丁二烯/烃混合物与一氧化碳和过量的C1 -C 4 - 链烷醇,(d)将所得反应混合物与其中所含的叔氮碱脱除,至每摩尔戊烯酸酯为0.1至0.3摩尔,过量 碳氢化合物和残留在反应混合物中的戊烯酸酯在羰基钴a存在下与一氧化碳和过量的C 1 -C 4烷醇反应 (e)反应混合物在步骤(b)中分离的酸性水溶液存在下用氧化剂处理,并将混合物分离成有机相 通过蒸馏分离丁二羧酸酯和水相,(f)水相用不与水混溶的溶剂萃取,分离相,所得水相脱离链烷醇和叔氮碱, 被回收到舞台(a)。