METHOD OF PREPARING AND RECOVERING 2-METHYL-5-IODOBENZOIC ACID
    4.
    发明公开
    METHOD OF PREPARING AND RECOVERING 2-METHYL-5-IODOBENZOIC ACID 审中-公开
    VERFAHREN ZUR HERSTELLUNG UNDRÜCKGEWINNUNGVON 2-METHYL-5-IODOBENZOESÄURE

    公开(公告)号:EP3059220A4

    公开(公告)日:2017-06-14

    申请号:EP13895696

    申请日:2013-10-18

    IPC分类号: C07C51/363 C07C63/70

    CPC分类号: C07C51/363 C07C63/70

    摘要: Provided is a method of preparing and recovering 2-methyl-5-iodobenzoic acid. The method utilizes o-methylbenzoic acid as raw material, iodinating via iodine/potassium persulfate in a mixed acid solvent to obtain a mixture of 2-methyl-5-iodobenzoic acid, 2-methyl-3-iodobenzoic acid, and 2-methyl-3, 5-diiodobenzoic acid; refining to obtain 2-methyl-5-iodobenzoic acid and recoverable mother liquor, the recoverable mother liquor being a mixture of 2-methyl-5-iodobenzoic acid, 2-methyl-3-iodobenzoic acid, and 2-methyl-3, 5-diiodobenzoic acid; conducting catalytic hydrogenation and deiodination to recover o-methylbenzoic acid and iodide ions; and oxidating the iodide ions to recover iodine. The whole process is recycled. The preparation and recovery method has cheap and easily available raw materials, and is easy of operation, has low requirements for equipment, and is suitable for large-scale industrial production.

    摘要翻译: 提供了一种制备和回收2-甲基-5-碘苯甲酸的方法。 该方法以邻甲基苯甲酸为原料,通过碘/过硫酸钾在混合酸溶剂中碘化,得到2-甲基-5-碘苯甲酸,2-甲基-3-碘苯甲酸和2-甲基-3-碘苯甲酸的混合物, 3,5-二碘苯甲酸; 精制以获得2-甲基-5-碘苯甲酸和可回收母液,所述可回收母液为2-甲基-5-碘苯甲酸,2-甲基-3-碘苯甲酸和2-甲基-3,5 - 二碘苯甲酸; 进行催化氢化和脱碘以回收邻甲基苯甲酸和碘离子; 并氧化碘离子以回收碘。 整个过程被回收。 该制备和回收方法原料廉价易得,操作简单,对设备要求低,适合大规模工业化生产。

    TRANSVINYLIERUNG ALS ERSTE STUFE EINER KOPPELPRODUKTION VON VINYLESTERN UND ESSIGSÄURE- ODER PROPIONSÄUREFOLGEPRODUKTEN
    7.
    发明公开
    TRANSVINYLIERUNG ALS ERSTE STUFE EINER KOPPELPRODUKTION VON VINYLESTERN UND ESSIGSÄURE- ODER PROPIONSÄUREFOLGEPRODUKTEN 有权
    转载请注明出处:EINER KOPPELPRODUKTION VON VINYLESTERN UNDESSIGSÄURE-ODERPROPIONSÄUREFOLGEPRODUKTEN

    公开(公告)号:EP2812306A1

    公开(公告)日:2014-12-17

    申请号:EP13700621.9

    申请日:2013-01-18

    申请人: OXEA GmbH

    摘要: The invention relates to a method for the coupling production of acetic acid or propionic acid reaction products and a vinyl ester of formula R-C(O)O-CH = CH2
    by a transvinylation reaction of a carboxylic acid of formula R-C(O)OH with a transvinylation reagent of formula R
    1 -C(O)O-CH = CH
    2 wherein R represents an aliphatic, cycloaliphatic or aromatic radical and R
    1 is methyl or ethyl and the transvinylation reaction is continuously carried out without removing a reaction partner in the presence of a transition metal catalyst containing at least one transition metal selected from the group comprising ruthenium, osmium, rhodium, iridium, palladium and platinum, the obtained reaction mixture being separated from its components, the vinyl ester of formula R-C(O)O-CH = CH2 and the carboxylic acid of formula R
    1 -C(O)-OH being separated and the thus obtained carboxylic acid R
    1 -C(O)-OH being converted into a derivative of formula R
    1 -C(O)-X, R
    1 -CH
    2 -OH or R
    6 -C(O)-OH.

    摘要翻译: 通过式R-C(O)OH的羧酸与式R1-C(O)的转乙烯化试剂的反式化反应共同制备式R-C(O)O-CH = CH 2的乙烯基酯的方法 )O-CH = CH 2,其特征在于:(a)在90至160℃的温度和0.5至15MPa的压力下连续进行转化反应,而不会在过渡金属存在下撤离反应物 含有选自钌,锇,铑,铱,钯和铂中的至少一种过渡金属的催化剂; (b)将所得反应混合物分离成其组分,并且除去式R-C(O)O-CH = CH 2的乙烯基酯和式R 1 -C(O)-OH的羧酸; 和(c)将步骤(b)后获得的羧酸转化为其中X为乙烯氧基的式R 1 -C(O)-X,R 1 -CH 2 -OH或R 6 -C(O)-OH的衍生物, O-CH = CH 2,卤素,式OR 2的烷氧基,其中R 2是取代或未取代的具有1至10个碳原子的烃基,式NR 3 R 4的氨基,其中R 3和R 4各自独立地为氢或取代或未取代的烃基 具有1至10个碳原子的基团,或其中R 5是氢的式O-C(O)-R 5的羧基或具有1至10个碳原子的取代或未取代的烃基,R 6是部分或全部卤素取代的 R1激进。

    ELUENT SOLUTION
    8.
    发明公开
    ELUENT SOLUTION 有权
    ELUIERUNGSLÖSUNG

    公开(公告)号:EP2658831A1

    公开(公告)日:2013-11-06

    申请号:EP11808853.3

    申请日:2011-12-21

    IPC分类号: C07B59/00

    摘要: The present invention provides a novel method for the preparation of
    18 F-fluoride (
    18 F) for use in radiofluorination reactions. The method of the invention finds use especially in the preparation of
    18 F-labelled positron emission tomography (PET) tracers. The method of the invention is particularly advantageous where bulk solutions are prepared and stored in prefilled vials rather than being freshly prepared on the day of synthesis. Also provided by the present invention is a radiofluorination reaction which comprises the method of the invention, as well as a cassette for use in carrying out the method of the invention and/or the radiofluorination method of the invention on an automated radiosynthesis apparatus.

    摘要翻译: 本发明提供了一种用于制备用于放射性氟化反应的18F-氟化物(18F)的新方法。 本发明的方法特别用于制备18F标记的正电子发射断层扫描(PET)示踪剂。 本发明的方法特别有利的是,其中本体溶液被制备并储存在预填充小瓶中,而不是在合成当天新鲜制备。 本发明还提供了一种放射性氟化反应,其包括本发明的方法,以及用于在自动放射合成装置上实施本发明的方法和/或本发明的放射性氟化方法的盒。

    Process for producing 4-methyl-2,3,5,6-tetrafluorobenzyl alcohol
    9.
    发明公开
    Process for producing 4-methyl-2,3,5,6-tetrafluorobenzyl alcohol 有权
    Verfahren zur Herstellung von 4-甲基-2,3,5,6-四氟苄醇

    公开(公告)号:EP2471766A1

    公开(公告)日:2012-07-04

    申请号:EP12161764.1

    申请日:2008-02-14

    发明人: Hagiya, Koji

    摘要: A process for producing 4-methyl-2,3,5,6-tetrafluorobenzyl alcohol comprising the following steps (A) to (D):
    Step (A): a step for fluorinating 2,3,5,6-tetrachloroterephthaloyl dichloride to obtain tetrafluoroterephthaloyl difluoride,
    Step (B): a step for reducing tetrafluoroterephthaloyl difluoride to obtain 2,3,5,6-tetrafluoro-1,4-benzenedimethanol,
    Step (C): a step for chlorinating the 2,3,5,6-tetrafluoro-1,4-benzenedimethanol to obtain 4-chloromethyl-2,3,5,6-tetrafluorobenzyl alcohol,
    Step (D): a step for hydrogenating the 4-chloromethyl-2,3,5,6-tetrafluorobenzyl alcohol.

    摘要翻译: 一种制备4-甲基-2,3,5,6-四氟苄醇的方法,包括以下步骤(A)至(D):步骤(A):将2,3,5,6-四氯对苯二甲酰氯氟化为 获得四氟对苯二甲酰二氟,步骤(B):减少四氟对苯二甲酰二氟以获得2,3,5,6-四氟-1,4-苯二甲醇的步骤,步骤(C):将2,3,5,6 - 四氟-1,4-苯二甲醇,得到4-氯甲基-2,3,5,6-四氟苄醇,工序(D):使4-氯甲基-2,3,5,6-四氟苄醇氢化的工序。