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    SYNTHETIC METHOD OF 9,9-BIS[4-(2-HYDROXYETHOXY)PHENYL]FLUORENE
    1.
    发明申请
    SYNTHETIC METHOD OF 9,9-BIS[4-(2-HYDROXYETHOXY)PHENYL]FLUORENE 有权

    公开(公告)号：US20220135509A1

    公开(公告)日：2022-05-05

    申请号：US17574334

    申请日：2022-01-12

    申请人： Zhejiang Zhongxin Fluoride Materials Co., Ltd.

    发明人： Qiliang YUAN ,  Dongdong JIANG ,  Ying WAN ,  Yonggen SHI ,  Pengfei XU ,  Haifeng CHEN

    IPC分类号： C07C41/30 ,  C07C41/40

    摘要： A synthetic method of 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene, belonging to the technical field of chemical synthesis. 9-fluorenone, phenoxyethanol, a catalyst and a cocatalyst are stiffed in an alkane solvent and heated until refluxing, the generated water is removed from the reaction solution via an azeotropic method while reacting, the reaction solution is diluted with water after the reaction is ended, uniformly stirred and cooled to separate out crystals and then filtered, a filter cake is rinsed and dried to obtain a 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene finished product; the filtered crystallization mother liquor is subjected to standing and layering, a water phase is removed, then an organic phase is distilled to recycle the alkane solvent, and the concentrate is rectified to recycle phenoxyethanol.

    Method for the work-up of a surfactant-containing reaction mixture
    4.
    发明授权
    Method for the work-up of a surfactant-containing reaction mixture 失效
    用于处理含表面活性剂的反应混合物的方法

    公开(公告)号：US5912390A

    公开(公告)日：1999-06-15

    申请号：US568055

    申请日：1995-12-06

    申请人： Ortwin Wagner ,  Reinhard Schomacker

    发明人： Ortwin Wagner ,  Reinhard Schomacker

    IPC分类号： B01D17/00 ,  B01D17/04 ,  C07B35/06 ,  C07B63/00 ,  C07C5/00 ,  C07C17/25 ,  C07C21/21 ,  C07C41/34 ,  C07C41/38 ,  C07C43/205 ,  C07C67/10 ,  C07C67/58 ,  C07C209/86 ,  C07C231/08 ,  C07C253/34 ,  C07C255/04 ,  C07C41/40

    CPC分类号： C07B63/00 ,  B01D17/042 ,  C07C41/16 ,  C07C41/34 ,  Y10S516/925

    摘要： A method for the work-up of a nonionic surfactant-containing microemulsion reaction mixture formed in the o-alkylation of phenols by an alkyl halide in the presence of sodium hydroxide. Said mixture has one reaction product present as an aqueous phase and a further reaction product present as a water immiscible phase and which the reaction mixture is obtained in microemulsion form. Said reaction mixture is worked up by:a) subjecting this microemulsion to a temperature decreased by 20 to 50K thereby forming an aqueous phase having a high surfactant content and a substantially surfactant-free organic phase,b) separating off the substantially surfactant-free organic phase formed and replacing said surfactant-free organic phase with an organic solution of the alkyl halide. After the replacement of the substantially surfactant-free phase,c) the reaction mixture thus treated is subjected to a temperature increase by 10 to 80K thereby forming a substantially surfactant-free aqueous phase and a high surfactant content organic phase,d) the substantially surfactant-free aqueous phase is separated off and replaced by additional aqueous solution of phenols. The mixture then present can be fed again to the reaction.

    摘要翻译： 一种用于在氢氧化钠存在下通过烷基卤在酚烷基化中形成的含非离子表面活性剂的微乳液反应混合物的处理方法。 所述混合物具有作为水相存在的一个反应产物和作为水不混溶相存在的另外的反应产物，并且反应混合物以微乳液形式获得。 所述反应混合物通过以下方法处理：a）使该微乳液的温度降低20至50K，从而形成具有高表面活性剂含量的水相和基本上不含表面活性剂的有机相，b）分离基本上无表面活性剂的有机物 用烷基卤的有机溶液形成和替代所述不含表面活性剂的有机相。 在更换基本不含表面活性剂的相后，c）将如此处理的反应混合物的温度升高10至80K，从而形成基本上不含表面活性剂的水相和高表面活性剂含量的有机相，d）基本上表面活性剂 分离出无水相并用另外的酚类水溶液代替。 然后存在的混合物可以再次进料到反应中。

    Method of purifying acifluorfen
    6.
    发明授权
    Method of purifying acifluorfen 失效
    三氟化合物的净化方法

    公开(公告)号：US5446197A

    公开(公告)日：1995-08-29

    申请号：US78993

    申请日：1993-06-17

    申请人： Mark Sandison ,  Ron Eva ,  Lawrence E. James

    发明人： Mark Sandison ,  Ron Eva ,  Lawrence E. James

    IPC分类号： C07C41/40 ,  C07C43/257 ,  C07C43/275 ,  C07C43/285 ,  C07C43/29 ,  C07C201/16 ,  C07C205/59 ,  C07C205/00

    CPC分类号： C07C201/16

    摘要： A method of purifying acifluorfen to achieve a purity of greater than about 85% by weight involves heating to dissolution a solution of an acifluorfen crude wet cake and at least one solvent from the group of 1,2-dichlorobenzene, monochlorobenzene, o-xylene and p-xylene, with the solution having from about 10 to about 30 weight percent of acifluorfen crude wet cake. The-solution is then cooled until crystals of purified acifluorfen form. The crystals are then filtered at a temperature within the range of from about 0.degree. to about 30.degree. C. The filtered crystals are then recovered.

    摘要翻译： 净化三氟果霜以达到大于约85重量％的纯度的方法涉及加热溶解氟锁草醚粗湿滤饼和至少一种来自1,2-二氯苯，一氯苯，邻二甲苯和 对二甲苯，溶液具有约10至约30重量％的三氟果霜粗湿饼。 然后将溶液冷却至纯化的三氟果霜形成晶体。 然后将晶体在约0℃至约30℃的温度范围内过滤。然后回收过滤的晶体。

    Process for the preparation of 4,4'-dihydroxydiphenyl ether
    7.
    发明授权
    Process for the preparation of 4,4'-dihydroxydiphenyl ether 失效
    制备4,4'-二羟基二苯醚的方法

    公开(公告)号：US4675457A

    公开(公告)日：1987-06-23

    申请号：US906995

    申请日：1986-09-12

    申请人： Edgar Vorwerk

    发明人： Edgar Vorwerk

    IPC分类号： C07C41/09 ,  C07C41/34 ,  C07C43/295 ,  C07C41/40

    CPC分类号： C07C41/34 ,  C07C41/09 ,  C07C43/295

    摘要： The invention relates to a process for the preparation of 4,4'-dihydroxydiphenyl ether by dehydration of hydroquinone using sulfonic acids or sulfuric acid as catalysts at elevated temperatures. The dehydration product is stirred with an excess of water at 80.degree. to 110.degree. C. The higher condensed byproducts which are undissolved during this are separated off, and the ether desired is allowed to crystallize out of the filtrate obtained.

    摘要翻译： 本发明涉及通过在高温下使用磺酸或硫酸作为催化剂脱氢氢醌来制备4,4'-二羟基二苯醚的方法。 脱水产物在80-110℃下用过量的水搅拌。分离出未溶解的较高浓缩副产物，所需的乙醚从得到的滤液中结晶出来。

    Process for the preparation of a very pure commercial form of 4,2',4'-trichloro-2-hydroxydiphenyl ether
    8.
    发明授权
    Process for the preparation of a very pure commercial form of 4,2',4'-trichloro-2-hydroxydiphenyl ether 失效
    用于制备非常纯的商业形式的4,2'，4'-三氯-2-羟基二苯醚的方法

    公开(公告)号：US4490562A

    公开(公告)日：1984-12-25

    申请号：US462258

    申请日：1983-01-31

    申请人： Werner Schreiber ,  Michael Marky

    发明人： Werner Schreiber ,  Michael Marky

    IPC分类号： C07C41/30 ,  C07C41/00 ,  C07C41/26 ,  C07C41/34 ,  C07C41/40 ,  C07C43/295 ,  C07C67/00 ,  C07C41/38 ,  C07C41/42

    CPC分类号： C07C41/26 ,  C07C41/38 ,  C07C41/40

    摘要： A very pure, dust-free commercial form of 4,2',4'-trichloro-2-hydroxydiphenyl ether with little odor is prepared by diazotizing 4,2'4'-trichloro-2-aminodiphenyl ether, boiling the diazonium salt and purifying the reaction product. The pure, dust-free and odor-free commercial form is obtained by separating off the acid aqueous phase of the reaction mixture, rendering the mixture containing 4,2'4'-trichloro-2-hydroxydiphenyl ether and 2,4,8-trichlorodibenzofuran alkaline, extracting it several times with an inert water-immiscible solvent, either after removal of the organic solvent by steam distillation and precipitation of the by-product 2,4,8-trichlorodibenzofuran or directly, and then adjusting the pH to 3 to 10; subsequently, the highly volatile constituents are removed from the 4,2',4'-trichloro-2-hydroxydiphenyl ether melt which has separated out, the melt is subjected to molecular distillation and the distilled melt is introduced into an aqueous dispersion of crystalline 4,2',4'-trichloro-2-hydroxydiphenyl ether, this dispersion simultaneously being subjected to wet grinding. Filtration and drying gives a granular-like ready-to-use commercial form.

    摘要翻译： 通过重氮化4,2'4'-三氯-2-氨基二苯醚，沸腾重氮盐和重氮化物制备非常纯净，无尘的商业形式的4,2'，4'-三氯-2-羟基二苯醚， 纯化反应产物。 通过分离出反应混合物的酸性水相，得到纯的无尘，无臭味的商业形式，使含有4,2'-四氯-2-羟基二苯醚和2,4,8-三氯-2-羟基二苯醚的混合物， 三氯二苯并呋喃碱性，用惰性水不混溶溶剂萃取数次，无论是通过蒸汽蒸馏除去有机溶剂并沉淀副产物2,4,8-三氯二苯并呋喃或直接，然后将pH调节至3〜 10; 随后，从分离出的4,2'，4'-三氯-2-羟基二苯醚熔体中除去高挥发性成分，熔融物进行分子蒸馏，将蒸馏的熔体引入结晶4的水分散体 ，2'，4'-三氯-2-羟基二苯醚，该分散体同时进行湿磨。 过滤和干燥得到颗粒状的即用型商业形式。

    Method of stabilizing reduced coenzyme Q10
    10.
    发明授权
    Method of stabilizing reduced coenzyme Q10 有权
    稳定还原型辅酶Q10的方法

    公开(公告)号：US09532957B2

    公开(公告)日：2017-01-03

    申请号：US14197347

    申请日：2014-03-05

    申请人： Kaneka Corporation

    发明人： Takahiro Ueda ,  Tadao Ono ,  Mitsutoshi Moro ,  Shiro Kitamura ,  Yasuyoshi Ueda

    IPC分类号： A61K31/122 ,  A61K47/10 ,  A61K47/12 ,  A61K47/14 ,  A61K47/22 ,  B01D9/00 ,  C07C41/26 ,  C07C41/40 ,  C07C41/46 ,  C07C43/23 ,  A61K9/48

    CPC分类号： A61K31/122 ,  A61K9/4866 ,  A61K47/10 ,  A61K47/12 ,  A61K47/14 ,  A61K47/22 ,  B01D9/00 ,  C07C41/26 ,  C07C41/40 ,  C07C41/46 ,  C07C43/23

    摘要： The present invention provides a stabilization method, a preservation method and the like method of reduced coenzyme Q10, which is useful as functional nutritive foods, specific health foods and the like. Furthermore, the present invention provides a method for efficiently obtaining reduced coenzyme Q10 of high quality and by a method suitable for a commercial production. It is possible to handle and stably preserve reduced coenzyme Q10 under a condition that oxidation by a molecular oxygen is inhibited by contacting reduced coenzyme Q10 with, an ascorbic acid and citric acid or a related compound thereof, and thus a stabilized composition is obtained. Moreover, reduced coenzyme Q10 is converted into a crystalline state in such a condition that the formation of oxidized coenzyme Q10 as a byproduct is minimized by crystallizing reduced coenzyme Q10 in the presence of ascorbic acid or a related compound thereof etc., and thus a reduced coenzyme Q10 crystal of high quality is produced. Furthermore, by successively crystallizing the generated reduced coenzyme Q10 in the presence of ascorbic acid or related compound thereof after reducing oxidized coenzyme Q10 to reduced coenzyme Q10 using ascorbic acid or a related compound thereof, operations are simplified and minimized, and thus reduced coenzyme Q10 of high quality is produced.

    摘要翻译： 本发明提供还原型辅酶Q10的稳定化方法，保存方法等，其作为功能性营养食品，特定健康食品等有用。 此外，本发明提供了一种有效地获得高质量的还原型辅酶Q10的方法，以及适用于商业生产的方法。 在减少的辅酶Q10与抗坏血酸和柠檬酸或其相关化合物接触的条件下，通过分子氧的氧化被抑制，可以处理和稳定地保存还原型辅酶Q10，从而获得稳定的组合物。 此外，将还原型辅酶Q10转化为结晶状态，使得在抗坏血酸或其相关化合物等存在下使还原型辅酶Q10结晶化，从而使作为副产物的氧化型辅酶Q10的形成最小化， 生产高品质的辅酶Q10晶体。 此外，通过使用抗坏血酸或其相关化合物将氧化型辅酶Q 10还原为还原型辅酶Q10后，在抗坏血酸或其相关化合物存在下，依次结晶生成的还原型辅酶Q10，操作简化，最小化，因此减少了辅酶Q10 生产高品质。