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    Water miscible solvent based process for purifying a bisphosphate
    5.
    发明授权
    Water miscible solvent based process for purifying a bisphosphate 有权
    用于纯化二磷酸的水混溶溶剂基方法

    公开(公告)号：US08299149B2

    公开(公告)日：2012-10-30

    申请号：US13133346

    申请日：2009-12-21

    申请人： Joseph Zilberman ,  Dorit Canfi ,  Andrew Gregor ,  Andrew Piotrowski

    发明人： Joseph Zilberman ,  Dorit Canfi ,  Andrew Gregor ,  Andrew Piotrowski

    IPC分类号： C08K5/523

    CPC分类号： C07F9/12 ,  C08K5/523 ,  C09K21/12

    摘要： There is provided herein a process for purifying bisphosphate comprising solvating a molten bisphosphate in a mixture of water and water miscible solvent; cooling the solution over a period and to a temperature that provides for crystallization of solid product; increasing the pH of the solution prior to, and/or during, and/or after the initiation of crystallization, and/or after crystallization, by the addition of a base; and after crystallization is complete, separating solid product from the solution; washing the separated solid product in the same and/or different mixture of water and water miscible solvent; and, washing the solid product which has been washed in the mixture with water.

    摘要翻译： 本文提供了一种纯化二磷酸盐的方法，其包括在水和水混溶性溶剂的混合物中溶解熔融的二磷酸盐; 在一段时间内将溶液冷却至提供固体产物结晶的温度; 在结晶开始之前和/或期间和/或之后，和/或在结晶后，通过加入碱来增加溶液的pH值; 结晶完成后，将固体产物与溶液分离; 在与水和水混溶的溶剂的相同和/或不同混合物中洗涤分离的固体产物; 并且用水洗涤已经在混合物中洗涤的固体产物。

    Processes for the preparation of 3-bromoanisole and 3-bromonitrobenzene
    8.
    发明授权
    Processes for the preparation of 3-bromoanisole and 3-bromonitrobenzene 有权
    制备3-溴苯甲醚和3-溴硝基苯的方法

    公开(公告)号：US06380440B1

    公开(公告)日：2002-04-30

    申请号：US09680961

    申请日：2000-10-05

    申请人： Mark Gelmont ,  Joseph Zilberman

    发明人： Mark Gelmont ,  Joseph Zilberman

    IPC分类号： C07C4100

    CPC分类号： C07C41/01 ,  C07C201/12 ,  C07C205/12 ,  C07C43/225

    摘要： Process for the preparation of 3-bromoanisole comprising methoxydenitrating 3-bromonitrobenzene in the presence of a phase-transfer catalyst (PTC), and the preparation of 3-bromonirtobenzene by the bromination of nitrobenzene with bromine in oleum. The methoxydenitration reagent in an alkali metal methoxide, which is selected from sodium methoxide and potassium methoxide. The amount of methoxide used is 1-1.5 mol per mol of 3-bromonitrobenzene. The alkali methoxide can be a pre-prepared solid or it can be prepared in situ, by the reaction of the corresponding alkali hydroxide and methanol. In the case when pre-prepared solid methoxide is used, the effective amount of alkali hydroxide is between 1.2-1.7 mol per mol of 3-bromonitrobenzebe. The reaction temperatures are between about 40 to 80° C., with preference to reaction temperatures of 50 to 55° C. In the case in which methoxide is prepared in situ, the effective amount of alkali hydroxide is between 2.2-2.4 mol per mol of 3-bromonitrobenzene. The reaction temperatures are between about 50 to 80° C. with preference to reaction temperatures of 55 to 65° C.

    摘要翻译： 在相转移催化剂（PTC）的存在下，制备3-溴苯甲醚的方法，包括在3-溴硝基苯中甲氧基过氧化，通过在发烟硫酸中用溴溴化硝基苯来制备3-溴苯甲腈。 碱金属甲醇盐中的甲氧基浓缩试剂，其选自甲醇钠和甲醇钾。 所用的甲氧化物的量为每摩尔3-溴硝基苯为1-1.5摩尔。 碱金属甲醇盐可以是预制的固体，也可以通过相应的碱金属氢氧化物和甲醇的反应在原位制备。 在使用预制的固体甲醇钠的情况下，碱金属氢氧化物的有效量为每摩尔3-溴硝基苯醚为1.2-1.7摩尔。 反应温度为约40至80℃，优选反应温度为50至55℃。在原位制备甲醇钠的情况下，碱金属氢氧化物的有效量为2.2-2.4摩尔/摩尔 的3-溴硝基苯。 反应温度在约50至80℃之间，优选的反应温度为55至65℃。