Preparation of 2,2-disubstituted 3-chloropropionic esters
    2.
    发明授权
    Preparation of 2,2-disubstituted 3-chloropropionic esters 失效
    2,2-二取代的3-氯丙酸酯的制备

    公开(公告)号:US4837357A

    公开(公告)日:1989-06-06

    申请号:US111624

    申请日:1987-10-21

    摘要: 2,2-Disubstituted 3-chloropropionic esters I ##STR1## where R.sup.1 and R.sup.2 are each C.sub.1 -C.sub.6 -alkyl, C.sub.2 -C.sub.6 -oxaalkyl, C.sub.2 -C.sub.6 -alkenyl, C.sub.2 -C.sub.6 -oxaalkenyl, aryl or C.sub.7 -C.sub.12 -aralkyl or R.sup.1 -C-R.sup.2 is 5-, 6- or 7-membered ring, R.sup.3 is C.sub.2 -C.sub.6 -oxaalkyl, C.sub.2 -C.sub.6 -alkenyl, C.sub.2 -C.sub.6 -oxaalkenyl or C.sub.7 -C.sub.12 -aralkyl, are prepared by converting 2,2-disubstituted 3-hydroxypropanals II ##STR2## into the esterdiol III ##STR3## reacting this esterdiol III in the presence of a transesterification catalyst with an alcohol R.sup.3 OH to give the 3-hydroxyester IV ##STR4## reacting the hydroxyester IV with a stoichiometric or greater than stoichiometric amount of the thionyl chloride and thermally decomposing the product to give the chloropropionic ester I.

    摘要翻译: 2,2-二取代的3-氯丙酸酯I,其中R 1和R 2各自是C 1 -C 6 - 烷基,C 2 -C 6 - 氧杂烷基,C 2 -C 6 - 烯基,C 2 -C 6 - 氧杂链烯基,芳基或C 7 -C 12 - 芳烷基或R1-C-R2是5-,6-或7-元环,R3是C2-C6-氧杂烷基,C2-C6-烯基,C2-C6-氧杂链烯基或C7-C12-芳烷基,是通过将2 将2-二取代的3-羟基丙醛II转化成酯二醇III在酯交换催化剂与醇R 3 OH的存在下使该酯二醇III反应,得到3-羟基酯IV使羟基酯IV 化学计量或大于化学计量的亚硫酰氯,并热分解产物得到氯丙酸酯I.

    Recovery of trialkylamines and methyl formate from mixtures obtained in
the preparation of trimethylolalkanes
    6.
    发明授权
    Recovery of trialkylamines and methyl formate from mixtures obtained in the preparation of trimethylolalkanes 失效
    三氯甲烷制备中获得的混合物中的丙烯酰胺和甲基丙烯酸的回收

    公开(公告)号:US5149861A

    公开(公告)日:1992-09-22

    申请号:US664463

    申请日:1991-03-01

    CPC分类号: C07C29/88 C07C67/03

    摘要: Trialkylamines and methyl formate are recovered from reaction mixtures obtained in the preparation of trimethylolalkanes by reaction of n-alkanals with from 2.2 to 4.5 moles of formaldehyde in aqueous solution in the presence of from 0.6 to 3 mole of trialkylamine, each quantity based on 1 mole of alkanal, and subsequent hydrogenation in a process wherein the crude reaction mixturea) is heated to from 100.degree. to 200.degree. C., the water present in the reaction mixture is substantially separated off by distillation, together with any excess free trialkylamine, the trialkylamine present in the form of a trialkylammonium formate is freed to form a trimethylolalkane formate, the trialkylamine is distilled off and the trimethylolalkane formate is transesterified with methanol to trimethylolalkane and methyl formate in the presence or absence of a catalytic amount of an alkali metal alkoxide or alkaline earth metal alkoxide, orb) is substantially dewatered, any excess free trialkylamine being removed at the same time, the trialkylamine present in the form of a trialkylammonium formate is separated off by admixing the remaining mixture with methanol and heating the admixture to from 100.degree. to 200.degree. C. to form methyl formate and trialkylamine.

    摘要翻译: 三烷基胺和甲酸甲酯从制备三羟甲基烷烃得到的反应混合物中回收,通过在0.6至3摩尔三烷基胺存在的情况下,正链烷与2.2至4.5摩尔甲醛在水溶液中的反应,每个量基于1摩尔 然后在将粗反应混合物a)加热至100至200℃的过程中随后进行氢化,反应混合物中存在的水通过蒸馏与任何过量的游离三烷基胺基本上分离出来, 以三烷基铵甲酸盐形式存在的三烷基胺可以形成甲酸三羟甲基烷烃,在存在或不存在催化量的碱金属醇盐的条件下,将三烷基胺蒸馏除去,甲醇三甲氧基链烷烃甲酯与甲醇酯交换为三羟甲基烷烃和甲酸甲酯,或 碱土金属醇盐或b)基本脱水,任何过量游离的三烷基胺为 同时除去以三烷基甲酸铵形式存在的三烷基胺,通过将剩余的混合物与甲醇混合并将混合物加热至100至200℃以分离,形成甲酸甲酯和三烷基胺。

    Joint preparation of 3-dialkylaminopropionitriles, bis-(2-cyanoethyl)
ether and, if desired, ethylene-cyanohydrin
    7.
    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 poloxy-alkylene glycols
    10.
    发明授权
    Preparation of poloxy-alkylene glycols 失效
    烷氧基 - 亚烷基二醇的制备

    公开(公告)号:US5416240A

    公开(公告)日:1995-05-16

    申请号:US24903

    申请日:1993-03-02

    CPC分类号: C08G65/20

    摘要: Polyoxyalkylene glycols are prepared by a process in which tetrahydrofuran is polymerized with a total of not more than 95 mol %, based on the amount of tetrahydrofuran used, of one or more comonomers from the group consisting of the cyclic ethers and acetals in the absence of water and in the presence of a monohydric alcohol or of a monocarboxylic acid with the aid of an anhydrous heteropoly acid catalyst, and the polyoxyalkylene glycol is liberated from the resulting polyoxyalkylene glycol monoethers or polyoxyalkylene glycol monoesters by cleavage of the monoether or monoester bond.

    摘要翻译: 聚氧亚烷基二醇通过以下方法制备,其中四氢呋喃基于所用四氢呋喃的总量不超过95摩尔%,在不存在共聚单体的情况下聚合来自由环醚和缩醛组成的组中的一种或多种共聚单体 水和一元醇或单羧酸存在下,借助于无水杂多酸催化剂,通过裂解单醚或单酯键,从所得聚氧亚烷基二醇单醚或聚氧亚烷基二醇单酯中释放出聚氧亚烷基二醇。