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    • 3. 发明授权
    • Process for preparing higher unsaturated ketones
    • 制备高级不饱和酮的方法
    • US06300524B1
    • 2001-10-09
    • US09440281
    • 1999-11-15
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerUdo RheudeGerd KaibelThomas KrugLuise SpiskeHagen Jaedicke
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerUdo RheudeGerd KaibelThomas KrugLuise SpiskeHagen Jaedicke
    • C07C4500
    • C07C45/676Y02P20/582C07C49/255C07C49/203
    • The present invention relates to an improved process for preparing higher unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction , in a reactor system with fitted fractionation column, wherein A the &agr;,&bgr;-unsaturated alcohol is introduced into the reaction vessel together with the organic aluminum compound in the absence of effective amounts of a solvent, and the alkyl acetoacetate is metered into this mixture, B a reaction temperature which is as constant as possible at between 175° C. and 220° C., preferably between 180° C. and 200° C., is adjusted and C during the reaction the content of alkyl acetoacetate in the reaction mixture is adjusted to a value which is as constant as possible at between 1 and 3% by weight. It is advantageous in this process for the reaction temperature defined under B to be controlled by suitable variation of the heat input and/or by variation of the rate of addition of the alkyl acetoacetate, and for adequate mixing of the reaction mixture in the reaction vessel to be ensured This can be achieved with the aid of a stirrer, by pumping the reaction mixture through an external liquid circulation, by introducing the alkyl acetoacetate by means of a mixing nozzle or else by passing in a stream of inert gas. The process according to the invention is particularly suitable for the Carroll reaction of higher alcohols such as 3,7-dimethyl-1,6-octadien-3-ol (linalool), 3,7-dimethyl-1-octen-3-ol, 3,7,11-trimethyl-1,6,10-dodecatrien-3-ol (nerolidol), 3,7,11-trimethyl-1-dodecen-3-ol or 3,7,11-trimethyl-1,6-dodecadien-3-ol (dihydronerolidol).
    • 本发明涉及一种改进的制备高级不饱和酮的方法,该方法通过在具有合适分馏塔的反应器系统中,在卡罗尔反应中使相应的α,β-不饱和醇与烷基乙酰乙酸酯反应,其中引入α,β-不饱和醇 在没有有效量的溶剂的情况下,将有机铝化合物与有机铝化合物一起加入到反应容器中,并将乙酰乙酸烷基酯计量加入到该混合物中,B在175℃和220℃之间的反应温度尽可能恒定 在反应过程中,优选在180℃和200℃之间调节和C,将反应混合物中乙酰乙酸烷基酯的含量调节至1至3重量%之间尽可能恒定的值。 在该方法中,通过适当变化的热输入和/或通过烷基的加成速率的变化来控制在B下限定的反应温度, 乙酰乙酸酯,并使反应混合物在反应容器中充分混合以确保这可以借助于搅拌器,通过泵送反应混合物通过外部液体循环,通过引入烷基乙酰乙酸酯通过混合喷嘴 或者通过流入惰性气体流。根据本发明的方法特别适用于高级醇如3,7-二甲基-1,6-辛二烯-3-醇(芳樟醇),3, 7,7-二甲基-1-辛烯-3-醇,3,7,11-三甲基-1,6,10-十二碳三烯-3-醇(橙花叔醇),3,7,11-三甲基-1-十二碳烯-3-醇 或3,7,11-三甲基-1,6-十二碳二烯-3-醇(二氢吗啉醇)。
    • 4. 发明授权
    • Process for preparing unsaturated ketones
    • 制备不饱和酮的方法
    • US06307106B1
    • 2001-10-23
    • US09440280
    • 1999-11-15
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerGerd KaibelHagen Jaedicke
    • Carsten OostManfred StroezelHeinz EtzrodtDietmar WellerGerd KaibelHagen Jaedicke
    • C07C4500
    • C07C45/68B01J19/1881B01J31/0211B01J2219/00038Y02P20/582C07C49/203
    • An improved process for preparing lower unsaturated ketones by reacting the corresponding &agr;,&bgr;-unsaturated alcohols with alkyl acetoacetates in a Carroll reaction in the presence of from 0.1 to 5 mol %, based on the alkyl acetoacetate to be reacted, of an organic aluminum compound as catalyst with elimination and continuous removal by distillation of the alkanol eliminated during the reaction from the alkyl acetoacetate in a reactor system with a fitted fractionation column, wherein A an &agr;,&bgr;-unsaturated alcohol which boils below 140° C. is introduced, in the absence of effective amounts of a solvent, together with the organic aluminum compound into the reaction vessel, B a reaction temperature which is as constant as possible between 170° C. and 250° C. is set under elevated pressure, C at this temperature, the alkyl acetoacetate is metered into the mixture, obtained in A, of the &agr;,&bgr;-unsaturated alcohol and the organic aluminum compound, and D during the reaction the content of alkyl acetoacetate in the reaction mixture is set at a value which is as constant as possible between 0.1 and 10% by weight.
    • 一种改进的制备低级不饱和酮的方法,该方法通过在卡罗尔反应中使相应的α,β-不饱和醇与烷基乙酰乙酸酯在0.1至5摩尔%存在下反应的待反应的乙酰乙酸烷基酯的有机铝化合物 作为催化剂,在具有适合的分馏塔的反应器系统中通过蒸馏从乙酰乙酸烷基酯反应中消除的烷醇消除并连续除去,其中引入沸点低于140℃的α,β-不饱和醇,在 没有有效量的溶剂与有机铝化合物一起进入反应容器B中,在170℃和250℃之间的反应温度一直保持在升高的压力下,在此温度下, 将乙酰乙酸烷基酯计量加入到A,得自α,β-不饱和醇和有机铝化合物的混合物中,并且在反应期间将D 将反应混合物中乙酰乙酸烷基酯的含量设定为0.1至10重量%之间尽可能恒定的值。
    • 8. 发明授权
    • Preparation of saccharin
    • 糖精的制备
    • US4464537A
    • 1984-08-07
    • US320333
    • 1981-11-12
    • Peter TonneHagen Jaedicke
    • Peter TonneHagen Jaedicke
    • C07D275/06
    • C07D275/06
    • A process for the preparation of saccharin by reacting an aqueous hydrochloric acid solution of o-methoxycarbonylbenzenediazonium chloride with sulfur dioxide, wherein(a) the aqueous diazonium salt solution is reacted with sulfur dioxide at from 0.degree. to 100.degree. C. in the presence of a water-immiscible or only partially water-miscible inert organic solvent,(b) in order to decompose the diazonium salt, the reaction mixture is treated simultaneously or subsequently with a diazonium salt decomposition catalyst,(c) the aqueous organic reaction mixture, or the organic phase obtained after removing the aqueous phase, is treated with an oxidizing agent at from 0.degree. to 100.degree. C. and(d) the organic phase is reacted with aqueous ammonia at from 0.degree. to 50.degree. C. and the saccharin is isolated from the aqueous phase in a conventional manner by acidifying with a strong acid.
    • 通过使邻甲氧基羰基苯并重氮盐酸盐水溶液与二氧化硫反应来制备糖精的方法,其中(a)重氮盐水溶液与二氧化硫在0℃至100℃下,在 (b)为了分解重氮盐,将反应混合物同时或随后用重氮盐分解催化剂处理,或(c)含水有机反应混合物,或 除去水相后得到的有机相用0〜100℃的氧化剂处理。