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    Preparation of triethyl phosphate
    2.
    发明授权
    Preparation of triethyl phosphate 失效
    磷酸三乙酯的制备

    公开(公告)号：US06673955B2

    公开(公告)日：2004-01-06

    申请号：US10302543

    申请日：2002-11-22

    Applicant: Karl-Heinz Mitschke ,  Kaspar Hallenberger ,  Ottfried Schlak ,  Johannes Kaulen

    Inventor： Karl-Heinz Mitschke ,  Kaspar Hallenberger ,  Ottfried Schlak ,  Johannes Kaulen

    IPC: C07F902

    CPC classification number: C07F9/11

    Abstract: The invention relates to a process for preparing triethyl phosphate by reacting phosphorus oxychloride with a greater than stoichiometric quantity of ethanol under reduced pressure at temperatures of from 0 to 50° C. in a reaction vessel, wherein a) the volatile components resulting from the reaction are predominantly condensed by means of a reflux condenser and the remaining volatile components are passed into a scrubber filled with water, b) after the end of the reaction, the reaction mixture is separated distillatively in an outgassing column into a top product and a bottom product which predominantly comprises triethyl phosphate, c) the top product of the outgassing column is combined with the contents of the scrubber and d) the contents of the scrubber are separated distillatively in an azeotropic distillation to obtain water and ethanol as top product and the ethanol, preferably after dewatering, is preferably returned to the reaction.

    Abstract translation: 本发明涉及通过在反应容器中在0至50℃的温度下在减压下使磷酰氯与大于化学计量的乙醇反应来制备磷酸三乙酯的方法，其中a）由反应产生的挥发性组分为 主要通过回流冷凝器冷凝，剩余的挥发性成分进入填充有水的洗涤器，b）在反应结束后，将反应混合物在脱气塔中蒸馏分离成顶部产物和底部产物， 主要包括磷酸三乙酯，c）除气塔的顶部产物与洗涤器的内容物组合，d）洗涤器的内容物在共沸蒸馏中蒸馏分离，得到水和乙醇作为顶级产物和乙醇，优选在 脱水，优选返回到反应中。

    Optically active oxiranes
    3.
    发明授权
    Optically active oxiranes 失效
    光学活性环氧乙烷

    公开(公告)号：US4988823A

    公开(公告)日：1991-01-29

    申请号：US372062

    申请日：1989-06-27

    Applicant: Johannes Kaulen

    Inventor： Johannes Kaulen

    IPC: A01N43/24 ,  C07B53/00 ,  C07C45/00 ,  C07C47/273 ,  C07C67/00 ,  C07C309/65 ,  C07D249/08 ,  C07D411/04 ,  C07D521/00

    CPC classification number: C07D231/12 ,  C07D233/56 ,  C07D249/08 ,  C07D411/04

    Abstract: Optically active oxiranes of the formula ##STR1## in which R represents substituted or unsubstituted alkyl, substituted or unsubstituted cycloalkyl or represents substituted or unsubstituted phenyl, andR.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5 and R.sup.6 represent hydrogen or alkyl, at least one of the radicals representing alkyl, orR.sup.4 and R.sup.5 together represent alkanediyl, which is unsubstituted or substituted by alkyl, or R.sup.4 and R.sup.5 together with the adjacent carbon atoms represent a fused bicyclic hydrocarbon radical, which is unsubstituted or substituted by alkylare produced by reacting an enantiomerically pure oxathiane ketone of the formula ##STR2## with a sulphonium or sulphoxonium salt. The product can be converted to optically active 2-hydroxyethylazole derivatives of the formula ##STR3##

    Abstract translation: 式（I）的光学活性环氧乙烷，其中R表示取代或未取代的烷基，取代或未取代的环烷基或表示取代或未取代的苯基，且R 1，R 2，R 3，R 4，R 5和R 6表示氢或烷基， 代表烷基的至少一个基团，或者R 4和R 5一起表示未被取代或被烷基取代的烷二基，或者R4和R5与相邻的碳原子一起表示稠合的双环烃基，其未被取代或被烷基取代 通过将式（IMA）（II）的对映异构体纯的氧硫杂环己酮与锍盐或磺基锍盐反应。 该产物可以转化成式（VI）的光学活性2-羟基乙唑衍生物，

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