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    Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the purification thereof
    1.
    发明授权
    Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the purification thereof 失效
    6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物的制备方法及其纯化方法

    公开(公告)号：US4804755A

    公开(公告)日：1989-02-14

    申请号：US902427

    申请日：1986-08-29

    申请人： Dieter Reuschling ,  Adolf Linkies ,  Walter Reimann ,  Otto E. Schweikert ,  Karl E. Mack ,  Wolfgang Ebertz

    发明人： Dieter Reuschling ,  Adolf Linkies ,  Walter Reimann ,  Otto E. Schweikert ,  Karl E. Mack ,  Wolfgang Ebertz

    IPC分类号： A23L27/20 ,  A23L27/30 ,  C07D291/06

    CPC分类号： C07D291/06

    摘要： The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxothiazin-4-one 2,2-dioxide are prepared by cyclizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert inorganic solvent, hydrolyzing the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO3-adduct after the cyclization reaction, in the event that the amount of SO3 employed is more than equimolar, purifying the organic phase (which has separated out) by extraction with a small volume of water or dilute aqueous sulfuric acid, preferably only with water, and isolating, by neutralization with bases, the non-toxic salts of the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide from the organic phase thus purified.The said salts are obtained in this process in an extremely pure form; they are valuable synthetic sweetening agents. The potassium salt is known as acesulfam (K).

    摘要翻译： 6-甲基-3,4-二氢-1,2,3-氧代噻嗪-4-酮2,2-二氧化物的无毒盐通过将乙酰乙酰胺-N-磺酸或其盐与至少大约 在与水不混溶的惰性有机溶剂存在下等摩尔量的SO 3，如果合适的话也可以是惰性无机溶剂，水解6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮 在环化反应后以SO 3 - 加合物的形式获得的二氧化二氮，在所用SO 3的量大于等摩尔的情况下，通过用少量体积的萃取纯化有机相（其分离出来） 水或稀硫酸水溶液，优选仅用水，并通过与碱中和，分离出6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2的无毒盐， 从有机相中纯化二氧化碳。 所述盐在该方法中以非常纯的形式获得; 它们是有价值的合成甜味剂。 钾盐被称为乙酰磺胺酸（K）。

    Process for the manufacture of resorcinols from .delta.-ketocarboxylic acid esters
    2.
    发明授权
    Process for the manufacture of resorcinols from .delta.-ketocarboxylic acid esters 失效
    从α-酮羧酸酯制造间苯二酚的方法

    公开(公告)号：US4250336A

    公开(公告)日：1981-02-10

    申请号：US45941

    申请日：1979-06-06

    申请人： Werner H. Muller ,  Karl E. Mack ,  Hansjorg Hey

    发明人： Werner H. Muller ,  Karl E. Mack ,  Hansjorg Hey

    IPC分类号： C07C43/23 ,  B01J23/00 ,  C07C27/00 ,  C07C37/00 ,  C07C37/06 ,  C07C37/07 ,  C07C39/08 ,  C07C39/12 ,  C07C41/00 ,  C07C67/00

    CPC分类号： C07C37/07 ,  Y02P20/584

    摘要： Resorcinols are prepared by converting .delta.-ketocarboxylic acid esters in the gaseous phase at a temperature from 250.degree. to 500.degree. C. in the presence of hydrogen at a catalyst. The catalyst consists of two components which are prepared separately and combined thereafter. The first component contains at least one compound of a metal of group VIII and/or at least one compound of a metal of group I B supported on one or several carrier materials. The second component contains at least one compound of a metal of group II A and/or IV A and/or III B and/or IV B supported on one or several carrier materials. A particularly preferred catalyst consists of a mixture of equal volume parts of platinum/charcoal as first component and of thorium/charcoal as second component.

    摘要翻译： 在氢气存在下，在催化剂存在下，在250〜500℃的温度下，将气态的α-酮羧酸酯转化成间苯二酚。 催化剂由两种组分组成，分别制备，然后合并。 第一组分含有至少一种第一族金属化合物和/或至少一种负载在一种或多种载体材料上的至少一种I B族金属化合物。 第二组分包含至少一种负载在一种或多种载体材料上的IIA族和/或IVA族和/或IIIB族和/或IVB族金属的化合物。 特别优选的催化剂由等体积份量的铂/炭作为第一组分和作为第二组分的钍/炭的混合物组成。

    Preparation of acetoacetarylamides
    3.
    发明授权
    Preparation of acetoacetarylamides 失效
    乙酰乙酰胺的制备

    公开(公告)号：US5523486A

    公开(公告)日：1996-06-04

    申请号：US326100

    申请日：1994-10-19

    申请人： Karl E. Mack ,  Michael Bohusch

    发明人： Karl E. Mack ,  Michael Bohusch

    IPC分类号： C07C231/04 ,  C07C235/80

    CPC分类号： C07C231/04

    摘要： A process for preparing acetoacetarylamides of the formula I ##STR1## where R.sup.1 and R.sup.2 are identical or different alkyl radicals,l and m are each 0, 1 or 2, andis 0 or 1,by addition of diketene to the appropriate arylamine by continuously reacting the arylamine with diketene in the presence of a mixture of water and of a (C.sub.1 -C.sub.4)-alkanol at temperatures from 60.degree. C. to 100.degree. C. in the course of from 0.1 to 10 min.

    摘要翻译： 制备式I的乙酰乙酰胺的方法，其中R 1和R 2是相同或不同的烷基，l和m各自为0,1或2，并且为0或1，通过连续地向适当的芳基胺中加入双烯酮 在0.1至10分钟的过程中，在水和（C 1 -C 4） - 烷醇的混合物存在下，使芳基胺与双烯酮反应，其温度为60℃至100℃。

    Preparation of 5-acetoacetylamino-2-benzimidazolone
    4.
    发明授权
    Preparation of 5-acetoacetylamino-2-benzimidazolone 失效
    5-乙酰乙酰氨基-2-苯并咪唑酮的制备

    公开(公告)号：US5476948A

    公开(公告)日：1995-12-19

    申请号：US325780

    申请日：1994-10-19

    申请人： Karl E. Mack ,  Michael Bohusch

    发明人： Karl E. Mack ,  Michael Bohusch

    IPC分类号： C07D235/26 ,  C07D235/24

    CPC分类号： C07D235/26

    摘要： A process for preparing 5-acetoacetylamino-2-benzimidazolone by continuous reaction of 5-amino-2-benzimidazolone with diketene comprises carrying out the reaction in the presence of a water-soluble (C.sub.1 -C.sub.4)-alcohol or of a mixture of this alcohol with water at the boiling temperature.

    摘要翻译： 通过5-氨基-2-苯并咪唑酮与双烯酮的连续反应制备5-乙酰乙酰氨基-2-苯并咪唑酮的方法包括在水溶性（C 1 -C 4） - 醇或其混合物的存在下进行反应 酒精与沸腾温度的水。

    Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the purification thereof
    6.
    发明授权
    Process for the preparation of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide and for the purification thereof 失效
    6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物的制备方法及其纯化方法

    公开(公告)号：US4806639A

    公开(公告)日：1989-02-21

    申请号：US902206

    申请日：1986-08-29

    申请人： Dieter Reuschling ,  Adolf Linkies ,  Walter Reimann ,  Otto E. Schweikert ,  Karl E. Mack

    发明人： Dieter Reuschling ,  Adolf Linkies ,  Walter Reimann ,  Otto E. Schweikert ,  Karl E. Mack

    IPC分类号： A23L27/20 ,  A23L27/30 ,  C07D291/06

    CPC分类号： C07D291/06

    摘要： 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is prepared by cylcizing acetoacetamide-N-sulfonic acid or its salts with an at least approximately equimolar amount of SO.sub.3 in the presence of a water-immiscible, inert organic solvent and, if appropriate, also an inert, inorganic solvent. In the event that an equimolar amount of SO.sub.3 is employed, working up is effected by adding aqueous sulfuric acid when the cyclization reaction is complete; in the event that the amount of SO.sub.3 employed is more than equimolar, the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide obtained in the form of the SO.sub.3 -adduct is hydrolyzed by adding water or ice, whereby sulfuric acid is formed from the SO.sub.3 combined in the SO.sub.3 -adduct.The inert, organic solvent is then removed from the resulting multi-phase mixture by distillation, and the 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is obtained in a pure form from the remaining aqueous sulfuric acid phase by crystallization. Additionally, quite generally, crude 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2-dioxide is purified by recrystallization from aqueous sulfuric acid. The non-toxic salts of 6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one 2,2 dioxide--in particular the potassium salt--are valuable synthetic sweetening agents.

    摘要翻译： 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物是通过将乙酰乙酰胺-N-磺酸或其盐与至少约等摩尔量的SO 3进行环烷酸 存在不溶于水的惰性有机溶剂，并且如果合适，也是惰性的无机溶剂。 在使用等摩尔量的SO 3的情况下，当环化反应完成时，通过加入硫酸水溶液进行加工; 在使用的SO 3的量超过等摩尔的情况下，以SO 3加合物的形式获得的6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物 通过加入水或冰水解，从而在SO 3加合物中组合的SO 3形成硫酸。 然后通过蒸馏从所得多相混合物中除去惰性有机溶剂，并将6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物 通过结晶从剩余的硫酸水相中纯化形式。 另外，通常，通过从硫酸水溶液中重结晶来纯化粗制的6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮2,2-二氧化物。 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮二氧化物（特别是钾盐）的无毒盐是有价值的合成甜味剂。