PROCESS FOR MANUFACTURING DISULFONIC ACID COMPOUND, ASYMMETRIC MANNICH CATALST, PROCESS FOR MANUFACTURING BETA-AMINOCARBONYL DERIVATIVE, AND NOVEL DISULFONATE
    3.
    发明申请
    PROCESS FOR MANUFACTURING DISULFONIC ACID COMPOUND, ASYMMETRIC MANNICH CATALST, PROCESS FOR MANUFACTURING BETA-AMINOCARBONYL DERIVATIVE, AND NOVEL DISULFONATE 审中-公开
    制备异氰酸酯化合物的方法,不对称催化剂,制备氨基甲酰胺衍生物和新型磺酸盐的方法

    公开(公告)号:US20100249431A1

    公开(公告)日:2010-09-30

    申请号:US12734284

    申请日:2008-10-01

    摘要: Hexamethylphosphoramide (HMPA) was added to a reaction vessel containing (R)-1,1′-binaphthyl-2,2′-dithiol and potassium hydroxide. The vessel was purged with oxygen and stirred at 80° C. for 5 days under 7 atmospheres of oxygen. After being cooled to room temperature, the reaction product was purified to yield potassium (R)-1,1′-binaphthyl-2,2′-disulfonate. The (R)-1,1′-binaphthyl-2,2′-disulfonic acid obtained from the disulfonate and 2,6-diphenylpyridine were stirred in acetonitrile, and then the solvent was evaporated under reduced pressure. Subsequently, magnesium sulfate and distilled CH2Cl2 were added to the reaction product, and the mixture was stirred at room temperature for 30 minutes. The resulting solution was cooled to 0° C. Benzaldehyde imine whose nitrogen is protected with Cbz and subsequently acetyl acetone were dropped into the solution over a period of 1 hour. The resulting mixture was further stirred at 0° C. for 30 minutes. A corresponding β-aminocarbonyl derivative was thus produced with an yield of 91% and an enantiomeric excess of 90% ee.

    摘要翻译: 将六甲基磷酰胺(HMPA)加入到含有(R)-1,1'-联萘-2,2'-二硫醇和氢氧化钾的反应容器中。 用氧气吹扫容器,并在7大气压的氧气下在80℃下搅拌5天​​。 冷却至室温后,将反应产物纯化,得到(R)-1,1'-联萘-2,2'-二磺酸钾。 从二磺酸和2,6-二苯基吡啶得到的(R)-1,1'-联萘-2,2'-二磺酸在乙腈中搅拌,然后减压蒸发溶剂。 随后,将硫酸镁和蒸馏的CH 2 Cl 2加入到反应产物中,并将混合物在室温下搅拌30分钟。 将所得溶液冷却至0℃。用Cbz和随后的乙酰丙酮保护其氮气的苯甲醛亚胺在1小时内滴加到溶液中。 将所得混合物在0℃下进一步搅拌30分钟。 因此产生相应的β-氨基羰基衍生物,产率为91%,对映体过量为90%ee。

    Polymer-supported arylbis(perfluoroalkylsulfonyl)-methane
    4.
    发明授权
    Polymer-supported arylbis(perfluoroalkylsulfonyl)-methane 失效
    聚合物负载的芳基双(全氟烷基磺酰基) - 甲烷

    公开(公告)号:US07026409B2

    公开(公告)日:2006-04-11

    申请号:US10471447

    申请日:2002-03-12

    IPC分类号: C08C19/20

    摘要: The present invention provides a solid acid catalyst that is excellent from the point of toxicity, environment and others, wherein reaction can be progressed effectively with Bronsted acid or Lewis acid catalyst. For example, the benzoylation reaction of alcohol can also be progressed easily, and further, the catalyst can be recovered and recycled easily. The para position of arylbis(perfluoroalkylsulfonyl)methane represented by the general formula [1] (wherein R1 shows a substituted or unsubstituted aryl group, Rf1 and Rf2 are independent to each other and show a perfluoroalkyl group), a pentafluorophenylbis(perfluoroalkylsulfonyl)methane, for example, is supported on a polystyrene resin, and a polystyrene-supported arylbis(perfluoroalkylsulfonyl)methane represented by the general formula [3] (wherein R3 shows a substituted or unsubstituted arylene group, Rf1 and Rf2 are the same as described above) is obtained.

    摘要翻译: 本发明提供从毒性,环境等方面优异的固体酸催化剂,其中可以使用布朗斯台德酸或路易斯酸催化剂有效地进行反应。 例如,醇的苯甲酰化反应也可以容易地进行,此外,可以容易地回收和回收催化剂。 由通式[1]表示的芳基双(全氟烷基磺酰基)甲烷的对位(其中R 1表示取代或未取代的芳基,Rf 1和R f) 2个彼此独立并且表示全氟烷基),五氟苯基双(全氟烷基磺酰基)甲烷例如负载在聚苯乙烯树脂上,由通式[D]表示的聚苯乙烯担载的芳基双(全氟烷基磺酰基)甲烷, 3](其中R 3表示取代或未取代的亚芳基,Rf 1和R 2 2与上述相同)。

    Process for production of amines
    9.
    发明申请
    Process for production of amines 有权
    胺的生产工艺

    公开(公告)号:US20070142639A1

    公开(公告)日:2007-06-21

    申请号:US10587279

    申请日:2005-01-26

    摘要: A process for producing an amine which is characterized by reacting an imine with a nucleophilic compound (except a trialkylsilyl vinyl ether) in the presence of a phosphoric acid derivative represented by the formula (1): wherein A1 represents a spacer; X1 and X2 represent each independently a divalent nonmetal atom or a divalent nonmetal atomic group; and Y1 is oxygen or sulfur. The invention provides a process by which amines (particularly optically active amines) useful as intermediates of medicines, agricultural chemicals, or the like can be produced without special post-treatment in high yield at high optical purity; and phosphoric acid derivatives (particularly optically active phosphoric acid derivatives) useful in the production of the amines.

    摘要翻译: 一种制备胺的方法,其特征在于在式(1)表示的磷酸衍生物存在下使亚胺与亲核化合物(三烷基甲硅烷基乙烯基醚除外)反应:其中A 1〜 代表间隔物; X 1和X 2各自独立地表示二价非金属原子或二价非金属原子团; 和Y 1是氧或硫。 本发明提供了一种以高光学纯度可高产率地用于药物,农药等作为中间体的胺(特别是光学活性胺)而不进行特殊后处理的方法。 和可用于制备胺的磷酸衍生物(特别是光学活性磷酸衍生物)。