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    PROCESS FOR PRODUCTION OF DISULFONIC ACID COMPOUND, ASYMMETRIC MANNICH CATALYST, PROCESS FOR PRODUCTION OF -AMINOCARBONYL DERIVATIVE, AND NOVEL DISULFONATE SALT
    4.
    发明公开
    PROCESS FOR PRODUCTION OF DISULFONIC ACID COMPOUND, ASYMMETRIC MANNICH CATALYST, PROCESS FOR PRODUCTION OF -AMINOCARBONYL DERIVATIVE, AND NOVEL DISULFONATE SALT 审中-公开
    制造方法DISCHWEFELSÄUREVERBINDUNG不对称曼尼希催化剂，用于生产？羰基衍生物和新颖DISULFONATSALZ

    公开(公告)号：EP2208722A1

    公开(公告)日：2010-07-21

    申请号：EP08843193.7

    申请日：2008-10-01

    申请人： National University Corporation Nagoya University

    发明人： ISHIHARA, Kazuaki ,  HATANO, Manabu ,  MAKI, Toshikatsu

    IPC分类号： C07C303/16 ,  B01J31/22 ,  C07C269/06 ,  C07C271/18 ,  C07C271/22 ,  C07C309/38 ,  C07D213/06 ,  C07D263/26 ,  C07B53/00 ,  C07B61/00

    CPC分类号： C07B53/00 ,  B01J31/0217 ,  B01J31/0225 ,  B01J31/0239 ,  B01J2231/346 ,  B01J2531/0266 ,  C07C269/06 ,  C07C303/16 ,  C07D213/06 ,  C07D263/26 ,  C07C271/18 ,  C07C271/22 ,  C07C309/35

    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 CH 2 Cl 2 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： 六甲基磷酰胺（HMPA），其加入到一个反应容器中包含（R）-1,1'-联萘-2,2'-二硫醇和氢氧化钾。 其中在氧气的7个大气压与氧气吹扫并搅拌在80℃下5天的容器中。 在冷却至室温后，将反应产物纯化，得到钾（R）-1,1'-联萘-2,2'-二磺酸。 的（R）-1,1'-联萘-2,2'-二磺酸与二磺酸和2,6- diphenylpyridines获得在乙腈，然后将溶剂减压蒸发。 随后，硫酸镁和蒸馏的CH 2 Cl 2中，加入到反应产物中，并且其在室温下搅拌30分钟该混合物。 将所得溶液冷却，其至0℃ 苯甲醛亚胺保护，Cbz基并随后乙酰丙酮其氮滴入该溶液在1小时的时间。 将得到的混合物，其在0℃下进一步搅拌30分钟。 相应²氨基羰基衍生物什么因此，在91％的产率，并在对映体过量为90％ee的与生产。