Process for preparing unsaturated ketones
    94.
    发明授权
    Process for preparing unsaturated ketones 失效
    制备不饱和酮的方法

    公开(公告)号:US06307106B1

    公开(公告)日:2001-10-23

    申请号:US09440280

    申请日:1999-11-15

    IPC分类号: C07C4500

    摘要: 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.

    摘要翻译: 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。

    Preparation of higher unsaturated ketones
    98.
    发明授权
    Preparation of higher unsaturated ketones 失效
    制备较高级的不饱和酮

    公开(公告)号:US4310705A

    公开(公告)日:1982-01-12

    申请号:US163401

    申请日:1980-06-26

    CPC分类号: C07C45/676

    摘要: An improved process for the preparation of higher unsaturated ketones, such as geranylacetone and farnesylacetone, by reacting a .beta.,.gamma.-unsaturated alcohol and an alkyl acetoacetate at an elevated temperature in the presence of an organic aluminum compound, with elimination, and removal, of the alcohol derived from the alkyl acetoacetate in a reactor system carrying a fractionating column. The improvement in the purity, yield, and especially space-time yield of the product is achieved by starting from an alcohol having a higher boiling point than that of the alkyl acetoacetate used, carrying out the reaction in the presence of a small amount of an inert liquid which has a boiling point between that of the alkyl acetoacetate and the alcohol to be eliminated therefrom, and ensuring that the temperature at the bottom of the fractionating column is only slightly higher than the boiling point of the added liquid, under the prevailing pressure.

    摘要翻译: 通过在有机铝化合物的存在下在升高的温度下使β,γ-不饱和醇和乙酰乙酸烷基酯反应来制备高级不饱和酮,如香叶基丙酮和法呢基丙酮的改进方法,消除和除去 在含有分馏塔的反应器系统中衍生自乙酰乙酸烷基酯的醇。 通过从具有比所用乙酰乙酸烷基酯的沸点高的醇开始的醇开始,在少量的存在下进行反应来实现产物的纯度,产率和特别的时空产率的改善 沸点在乙酰乙酸烷基酯和被除去的醇之间的沸点的惰性液体,并且确保分馏塔底部的温度仅略高于添加液体的沸点,在主要压力下 。

    Production of anhydrous or substantially anhydrous formic acid
    99.
    发明授权
    Production of anhydrous or substantially anhydrous formic acid 失效
    生产无水或基本无水的甲酸

    公开(公告)号:US4262140A

    公开(公告)日:1981-04-14

    申请号:US99760

    申请日:1979-12-03

    CPC分类号: C07C51/44 C07C51/09 C07C51/48

    摘要: A process for the production of anhydrous or substantially anhydrous formic acid by hydrolysis of methyl formate which is carried out in a column having an upper fractionating section, a middle hydrolysis section and a lower extraction section and in which(a) the hydrolysis is carried out in the middle section of the columm, with water and methyl formate in countercurrent,(b) the resulting formic acid is extracted, in the lower section of the column, by means of a carboxylic acid amide which is fed into the lower end of the middle section of the column,(c) the extract phase, consisting in the main of formic acid and the carboxylic acid amide, is distillatively dehydrated, or substantially dehydrated, in the lower section of the column,(d) the methanol and uncovered methyl formate are removed by fractional distillation in the upper section of the column and(e) the pure formic acid or concentrated aqueous formic acid is distilled from the anhydrous or substantially anhydrous extract phase in a second column, leaving the carboxylic acid amide.

    摘要翻译: 一种通过水解甲酸甲酯生产无水或基本上无水的甲酸的方法,该甲酸甲酯在具有上部分馏段,中间水解段和下部萃取段的塔中进行,其中(a)进行水解 在水的中间部分,与水和甲酸甲酯逆流,(b)所得甲酸在柱的下部通过羧酸酰胺萃取,该羧酸酰胺进料到 塔的中间部分,(c)主要由甲酸和羧酸酰胺组成的提取相在塔的下部进行蒸馏脱水或基本上脱水,(d)甲醇和未被覆盖的甲基 甲酸盐在塔的上部通过分馏除去,(e)从无水或基本上无水的提取物中蒸馏出纯甲酸或浓缩的甲酸水溶液 相在第二塔中,留下羧酸酰胺。