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    Method of preparing alkylisothiocyanic acid esters
    1.
    发明授权
    Method of preparing alkylisothiocyanic acid esters 失效
    制备碱性氨基酸酸酯的方法

    公开(公告)号：US5208361A

    公开(公告)日：1993-05-04

    申请号：US641260

    申请日：1991-01-15

    申请人： Gunter Giesselmann ,  Kurt Gunther

    发明人： Gunter Giesselmann ,  Kurt Gunther

    IPC分类号： C07C331/20

    CPC分类号： C07C331/20

    摘要： Alkylisothiocyanic acid esters having the formula R--N.dbd.C.dbd.S can be prepared by reacting N-alkyldithiocarbamates with hydrogen peroxide in aqueous phase at 95.degree. to 130.degree. C. The aqueous solution of N-alkyldithiocarbamate is reacted with a 20 to 40% by weight aqueous solution of hydrogen peroxide in a volumetric ratio of 1 to 0.8 to 1 while maintaining a pH of 1.5 to 4.5. The solutions are preferably sprayed into a reactor, at which time the alkylisothiocyanate formed distills off in vapor form and an aqueous phase containing the byproducts collects in the reactor. The method is capable of significantly increasing the space-time yield because much less sulfur is formed in comparison to the previously known method, which takes place at pH 5 to 9, thereby minimizing the shutdown times previously required for cleaning the reactor.

    摘要翻译： 具有式RN = C = S的烷基异硫氰酸酯可以通过N-烷基二硫代氨基甲酸酯与过氧化氢在95〜130℃的水相中反应来制备。N-烷基二硫代氨基甲酸酯水溶液与20〜40重量％ 过氧化氢水溶液，其体积比为1至0.8至1，同时保持pH为1.5至4.5。 溶液优选喷雾到反应器中，此时形成的异硫氰酸烷基酯以蒸气形式蒸馏出来，含有副产物的水相收集在反应器中。 与先前已知的在pH5至9下进行的方法相比，该方法能够显着增加空时产率，因为形成的硫少得多，从而使先前清洗反应器所需的关机时间最小化。

    Method and apparatus for the quantitative enrichment of volatile compounds by capillary distillation
    2.
    发明授权
    Method and apparatus for the quantitative enrichment of volatile compounds by capillary distillation 失效
    通过毛细管蒸馏定量浓缩挥发性化合物的方法和装置

    公开(公告)号：US5665208A

    公开(公告)日：1997-09-09

    申请号：US493083

    申请日：1995-06-21

    申请人： Gunter Giesselmann

    发明人： Gunter Giesselmann

    IPC分类号： B01D1/00 ,  B01D3/00 ,  B01D3/12

    CPC分类号： B01D3/12 ,  Y10S159/15 ,  Y10S159/28 ,  Y10S159/906

    摘要： A quantitative enrichment of volatile compounds from substances of the macro- to submicro field in a short time is realized by capillary distillation in a system which includes an evaporator vessel, on the bottom of which one or more filter plates are provided and which is connected to a condensing vessel by means of a capillary tube. The presence of filter plate(s) guarantees a uniform and constant boiling which facilitates the quantitative isolation of the volatile compounds.

    摘要翻译： 通过在包括蒸发器容器的系统中的毛细管蒸馏来实现在短时间内从宏观 - 亚微米场的物质定量富集挥发性化合物，其中底部设置有一个或多个过滤板，并连接到 冷凝容器通过毛细管。 过滤板的存在保证均匀且恒定的沸腾，这有助于挥发性化合物的定量分离。

    Process for the production of isothiocyanates
    4.
    发明授权
    Process for the production of isothiocyanates 失效
    异硫氰酸酯生产工艺

    公开(公告)号：US4089887A

    公开(公告)日：1978-05-16

    申请号：US762792

    申请日：1977-01-25

    申请人： Gunter Giesselmann ,  Gerd Schreyer ,  Rudolf Vanheertum

    发明人： Gunter Giesselmann ,  Gerd Schreyer ,  Rudolf Vanheertum

    IPC分类号： C01C3/20 ,  C07C331/16 ,  C07D277/38 ,  C07C161/04 ,  C07D211/98

    CPC分类号： C07C331/16

    摘要： Isothiocyanates of the formula (I)r -- n.dbd.c.dbd.s (i)in which R is a straight or branched alkyl group with 1 to 18 carbon atoms, preferably methyl, and wherein the alkyl group can be substituted once or more by --OH, --OR.sup.1 or --SR.sup.1 and where R.sup.1 is an alkyl group of 1 to 6 carbon atoms or R is cycloalkyl with 3 to 8 carbon atoms, benzyl or phenyl in which the aromatic nucleus can be substituted once or more by a chlorine atom, a bromine atom, a hydroxyl group, or --R.sup.1, --OR.sup.1 or --SR.sup.1 or R is a pyridyl or thiazolyl group prepared by reacting (1) a dithiocarbamate of the general formula (II) ##STR1## where R is as defined above and Me is an alkali atom, one valence of an alkaline earth metal atom or the ammonium group whose hydrogen atoms can be substituted by R with (2) a cyanogen halide, preferably cyanogen chloride, in the presence of water. There is employed one mole of a dithiocarbamate of formula II as a 5 to 50 weight % aqueous solution in the presence of an inert organic solvent which is not miscible with water, and preferably in the presence of a base at a temperature from about -10.degree. C to about +50.degree. C, preferably between 0.degree. C and 25.degree. C. There is employed at least one mole of cyanogen chloride per mole of dithiocarbamate. The isothiocyanate produced is isolated from the organic phase.

    摘要翻译： 式（I）R-N = C = S（I）的异硫氰酸酯，其中R是具有1至18个碳原子的直链或支链烷基，优选甲基，并且其中烷基可被一次或多次取代， OH，-OR1或-SR1，其中R1是1至6个碳原子的烷基或R是具有3至8个碳原子的环烷基，苄基或苯基，其中芳环可以被氯原子取代一次或多次， 溴原子，羟基或-R1，-OR1或-SR1或R是通过使（1）通式（II）的二硫代氨基甲酸酯（II）的反应制备的吡啶基或噻唑基，其中R为 Me是碱金属原子，一价碱土金属原子或其氢原子可被R取代的铵基，（2）卤化氰，优选氯化氰，在水存在下。 在惰性有机溶剂的存在下，使用1摩尔式II的二硫代氨基甲酸酯作为5至50重量％的水溶液，该惰性有机溶剂不与水混溶，优选在碱存在下，温度为约-10℃ ℃至约+ 50℃，优选0℃至25℃。每摩尔二硫代氨基甲酸盐使用至少1摩尔氯化氰。 所产生的异硫氰酸酯与有机相分离。