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    • 13. 发明授权
    • Preparation of .epsilon.-caprolactone
    • ε-己内酯的制备
    • US4341709A
    • 1982-07-27
    • US150260
    • 1980-05-15
    • Willi HofenHerbert KlenkGerd SchreyerOtto WeibergHelmut WaldmannHermann SeifertKarl-Hermann ReissingerWolfgang Swodenk
    • Willi HofenHerbert KlenkGerd SchreyerOtto WeibergHelmut WaldmannHermann SeifertKarl-Hermann ReissingerWolfgang Swodenk
    • C07D313/04C07D315/00C07D313/02
    • C07D315/00
    • A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.
    • 一种制备ε-己内酯的方法,包括:(a)使环己酮与过丙酸在有机溶剂中的溶液以环己酮的摩尔比约1.1-5:1的约0.1〜5:1的摩尔比在约10℃〜 形成基本上由ε-己内酯,丙酸和有机溶剂组成的反应混合物,(b)在第一蒸馏单元中将反应混合物从(a)中蒸馏,得到包含有机溶剂和蒸馏残余物的馏出物 (c)在一点将来自(b)的蒸馏残余物引入第二蒸馏单元以获得包含丙酸和未反应的环己酮的馏出物,从第二蒸馏单元彼此分离并在低于 引入第二蒸馏装置,ε-己内酯和任何高沸点组分,和(d)在第三蒸馏装置中蒸馏出馏出物(c)得到 基本上由丙酸组成的馏出物和包含丙酸和环己酮的混合物的蒸馏残渣。
    • 15. 发明授权
    • Production of .omega.-formyl carboxylic acid esters
    • 生产“7-甲酰基羧酸酯”
    • US4013709A
    • 1977-03-22
    • US651989
    • 1976-01-23
    • Helmut WaldmannWulf SchwerdtelWolfgang Swodenk
    • Helmut WaldmannWulf SchwerdtelWolfgang Swodenk
    • C07C69/67C07C67/00
    • C07C69/67
    • A process for the production of an .omega.-formyl carboxylic acid ester, comprising reacting an enol ether of a cyclic ketone with hydrogen peroxide in the presence of at least one catalyst selected from the group consisting of a compound of boron or of a metal of the Fifth or Sixth Secondary Group of the Periodic Table. Advantageously the enol ether has the formula ##STR1## wherein R.sub.1 is alkyl of 1 to about 3 carbon atoms, cycloalkyl of 5 or 6 carbon atoms or phenyl optionally substituted by fluorine, chlorine, alkoxy of 1 to about 3 carbon atoms, cyano or phenyl,n is an integer of about 3 to 10, andR.sub.2 each independently is hydrogen, fluorine, chlorine, cyano, alkoxy of 1 to about 4 carbon atoms, alkyl of 1 to about 6 carbon atoms, cycloalkyl of 5 to 7 carbon atoms or phenyl optionally substituted by fluorine, chlorine, cyano, alkoxy of 1 to about 4 carbon atoms or alkyl of 1 to about 6 carbon atoms,And the catalyst comprises about 15 to 25 mole % based on the hydrogen peroxide of a boron oxide, a boric acid, a salt of a boric acid, a boron halogen compound, a complex boron compound or a boric acid ester of the formula ##STR2## wherein R.sub.4, R.sub.5 and R.sub.6 each independently is alkyl of 1 to about 6 carbon atoms optionally substituted by hydroxyl, fluorine, chlorine, alkoxy of 1 to about 3 carbon atoms or phenyl, cycloalkyl of 5 to 7 carbon atoms or phenyl optionally substituted by fluorine, chlorine or alkyl of 1 to about 3 carbon atoms,Or about 0.01 to 1 mole % of at least one acetate, benzoate, acetylacetonate or naphthenate of a metal of the Fifth or Sixth Group of the Periodic table.