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    Continuous process for recovery of glycide
    2.
    发明授权
    Continuous process for recovery of glycide 失效
    持续的糖苷还原过程

    公开(公告)号：US4009188A

    公开(公告)日：1977-02-22

    申请号：US551015

    申请日：1975-02-19

    申请人： Wolfgang Heim ,  Axel Kleemann ,  Heinz Kolb ,  Gerd Schreyer

    发明人： Wolfgang Heim ,  Axel Kleemann ,  Heinz Kolb ,  Gerd Schreyer

    IPC分类号： C07D301/12 ,  C07D301/32 ,  B01D3/10 ,  B01D3/28

    CPC分类号： C07D301/32

    摘要： Glycide is prepared by reacting allyl alcohol with hydrogen peroxide in the presence of a tungsten compound as a catalysts the excess allyl alcohol and the greatest part of the water distilled off, the sump mixture obtained in the distillation is split at 110.degree.-220.degree. C. and 5 to 60 torr in a thin layer evaporator into a volatile portion which is predominantly glycide, high boiling by products and the residual part of the water and a sump portion of glycerine, polyglycerine and catalysts. The volatile liquid portion is broken into glycide, water and high boiling byproducts at 5 to 60 torr in a distillation apparatus directly connected to the thin layer evaporator.

    摘要翻译： 通过使烯丙醇与过氧化氢在钨化合物作为催化剂存在下制备过量的烯丙醇和蒸馏出的最大部分水，将蒸馏中获得的集水器混合物在110°-220℃ 和5至60托在薄层蒸发器中成为挥发性部分，其主要是糖苷，产物高沸点，剩余部分水和甘油，聚甘油和催化剂的贮槽部分。 在与薄层蒸发器直接连接的蒸馏装置中，挥发性液体部分在5至60托下破碎为糖，水和高沸点副产物。

    Production of 1-(3-hydroxy-propyl)-1,4-diazepane and 1,4-bis(3,4,5-trimethoxy-benzoyloxy)-propyl-diazepane derivatives thereof
    7.
    发明授权
    Production of 1-(3-hydroxy-propyl)-1,4-diazepane and 1,4-bis(3,4,5-trimethoxy-benzoyloxy)-propyl-diazepane derivatives thereof 失效
    1-（3-羟基 - 丙基）-1,4-二氮杂环庚烷和1,4-双（3,4,5-三甲氧基 - 苯甲酰氧基） - 丙基 - 二氮杂环庚烷衍生物的制备

    公开(公告)号：US4751298A

    公开(公告)日：1988-06-14

    申请号：US693344

    申请日：1985-01-22

    申请人： Axel Kleemann ,  Bernd Lehmann ,  Klaus Deller

    发明人： Axel Kleemann ,  Bernd Lehmann ,  Klaus Deller

    IPC分类号： A61K31/55 ,  B01J27/00 ,  C07B61/00 ,  C07C67/00 ,  C07C253/00 ,  C07C255/24 ,  C07D243/08

    CPC分类号： C07C255/00 ,  C07D243/08

    摘要： There is disclosed a process for the production of 1,4-bis-[3-(3,4,5-trimethoxybenzyloxy)-propyl]-diazepane which consists of first reacting 3-aminopropanol with acrylonitrile and subsequently reacting in aqueous solution with formaldehyde and hydrocyanic acid or with formaldehyde and an alkali cyanide in the presence of alkali hydrogen sulfite to form cyanomethyl-(2-cyano-ethyl)-(3-hydroxy-propyl)-amine; hydrogenating the thus obtained reaction product in the presence of a hydrogenating catalyst and ammonia to 1 (3-hydroxy-propyl)-1,4-diazepane and reacting the latter compound for example with 3-halogen propanol or with allyl alcohol and introducing two 3,4,5-trimethoxy-benzoyl groups into the thus obtained reaction product by esterification.

    摘要翻译： 公开了一种生产1,4-双[3-（3,4,5-三甲氧基苄氧基） - 丙基] - 二氮杂环丁烷的方法，该方法由首先使3-氨基丙醇与丙烯腈反应，随后在水溶液中与甲醛反应 和氢氰酸，或在碱金属亚硫酸盐存在下与甲醛和碱金属氰化物反应，形成氰基甲基 - （2-氰基 - 乙基） - （3-羟基 - 丙基） - 胺; 将由此得到的反应产物在氢化催化剂和氨的存在下氢化成1（3-羟基 - 丙基）-1,4-二氮杂环丁烷，并使后者化合物例如与3-卤素丙醇或烯丙醇反应并引入两个3 ，4,5-三甲氧基苯甲酰基通过酯化转化成如此得到的反应产物。

    Process for the production of non-aqueous hydrogen peroxide solutions and their use
    9.
    发明授权
    Process for the production of non-aqueous hydrogen peroxide solutions and their use 失效
    用于生产非水过氧化氢溶液及其用途的方法

    公开(公告)号：US4686010A

    公开(公告)日：1987-08-11

    申请号：US648137

    申请日：1984-09-07

    申请人： Karlheinz Drauz ,  Axel Kleemann

    发明人： Karlheinz Drauz ,  Axel Kleemann

    IPC分类号： C07C37/58 ,  B01J27/00 ,  C01B15/017 ,  C07C27/00 ,  C07C67/00 ,  B01D3/36

    CPC分类号： C01B15/017

    摘要： The production of solutions of hydrogen peroxide in phenol or its derivatives, e.g. hydrocarbyl substituted phenols, halo substituted phenols or phenol ethers, is carried out in a single step. Practically no loss of hydrogen peroxide occurs since a total distillation of hydrogen peroxide together with phenol or phenol derivative is avoided. Simultaneously the solutions obtained are practically free from water. The mixture of phenol or phenol derivative and aqueous hydrogen peroxide is treated with a material that boils below the boiling point of hydrogen peroxide, phenol or phenol derivative or forms an azeotrope with water that boils below the boiling point of hydrogen peroxide, phenol or phenol derivative and the water removed as an azeotrope. The solution of hydrogen peroxide in phenol or phenol derivative which remains behind is suitable for carrying out oxidation reactions and above all, also for hydroxylation reactions.

    摘要翻译： 生产苯酚或其衍生物中过氧化氢的溶液，例如 烃基取代的酚，卤代酚或苯酚醚在一个步骤中进行。 实际上不会发生过氧化氢的损失，因为避免了与苯酚或苯酚衍生物一起完全蒸馏过氧化氢。 同时获得的溶液实际上不含水。 苯酚或苯酚衍生物与过氧化氢水溶液的混合物用沸点低于过氧化氢，苯酚或苯酚衍生物的沸点的物质处理，或与沸点低于过氧化氢，苯酚或苯酚衍生物沸点的水形成共沸物 并将水作为共沸物除去。 过氧化氢在苯酚或苯酚衍生物中残留的溶液适用于进行氧化反应，尤其是羟基化反应。

    Process for the production of water-free organic hydrogen peroxide solution
    10.
    发明授权
    Process for the production of water-free organic hydrogen peroxide solution 失效
    生产无水有机过氧化氢溶液的方法

    公开(公告)号：US4564514A

    公开(公告)日：1986-01-14

    申请号：US510162

    申请日：1983-07-01

    申请人： Karlheinz Drauz ,  Axel Kleemann ,  Rolf Wirthwein

    发明人： Karlheinz Drauz ,  Axel Kleemann ,  Rolf Wirthwein

    IPC分类号： C01B15/017 ,  C01B15/023

    CPC分类号： C01B15/017

    摘要： The production of organic hydrogen peroxide solutions which are practically water-free until now has had the problem of either too high a water content of the solution or too great a loss of hydrogen peroxide through decomposition and passing over as distillate during the distillative drying. By selection of specific esters in combination with commensurately high pressures in the azeotropic removal of water, these disadvantages can be avoided. Extremely low water content solutions of hydrogen peroxide in high boiling solutions are produced by mixing hydrogen peroxide solutions in solvents whose azeotropic boiling point with water is below the boiling point of hydrogen peroxide with higher boiling solvents which form the highest azeotrope with water, whose boiling point is near or above the boiling point of hydrogen peroxide. Thereupon, the mixture is freed from both water and the lower boiling solvent. The mixture can be formed by an in situ method. Production of extremely low water containing solutions of hydrogen peroxide in high boiling solvents are produced by mixing hydrogen peroxide solutions in solvents whose azeotrope boiling point with water is below the boiling point of hydrogen peroxide with higher boiling solvents which form the highest azeotrope with water, whose boiling point is near or above the boiling point of hydrogen peroxide. Thereupon, the mixture is freed from both water and the lower boiling solvent. The above-mentioned mixture can also be produced by an in situ method.

    摘要翻译： 迄今为止几乎无水的有机过氧化氢溶液的生产具有溶液中水含量过高或分解过程中过氧化氢过多或蒸馏干燥过程中作为馏出物流失的问题。 通过选择特定的酯与共沸去除水中相当高的压力相结合，可以避免这些缺点。 过氧化氢在高沸点溶液中的极低含水量溶液是通过将过氧化氢溶液与共沸点与水低于过氧化氢沸点的溶剂混合，通过与沸水形成最高共沸物的较高沸点溶剂混合而制得的，其沸点 接近或高于过氧化氢的沸点。 因此，混合物从水和低沸点溶剂中释放出来。 混合物可以通过原位法形成。 在高沸点溶剂中生产极低含水量的过氧化氢的溶液是通过将过氧化氢溶液与沸点高于沸点溶剂的沸点高于沸点的溶剂在水中沸点高于沸点的溶剂混合， 沸点接近或高于过氧化氢的沸点。 因此，混合物从水和低沸点溶剂中释放出来。 上述混合物也可以通过原位法制备。