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2. 发明公开

EP0634409A1 Process of producing 2-cyano-4-oxo-4H-benzopyran compounds 失效转让
标题翻译： Verfahren zur Herstellung von 2-Cyano-4-Oxo-4H-Benzopyran Verbindungen。
公开(公告)号：EP0634409A1
公开(公告)日：1995-01-18
申请号：EP94110888.8
申请日：1994-07-13
申请人： SUMITOMO CHEMICAL COMPANY, LIMITED
发明人： Higashii, Takayuki , Ushio, Hideki , Fujimoto, Yukari , Matsumoto, Tsutomu , Minai, Masayoshi , Yasunaga, Katsuichi , Sogabe, Hiroshi , Kotera, Takahiro
IPC分类号： C07D311/24
CPC分类号： C07D311/24
摘要： There is disclosed a process of producing a 2-cyano-4-oxo-4H-benzopyran compound of the general formula (2):

wherein R¹ and R² are independently hydrogen, halogen, hydroxy, C₁-C₅ alkyl, C₁-C₅ alkoxy, nitro or a group of the RCONH wherein R is C₁-C₂₀ alkyl, phenyl, phenyl-substituted (C₁-C₂₀)alkyl, phenyl(C₁-C₂₀)alkoxyphenyl or (C₁-C₂₀)alkoxyphenyl. This production process is characterized in that a carboxamide of the general formula (1):

wherein R¹ and R² are each as defined above, is reacted with a dehydrating agent in the presence of a pyridine compound of the general formula (4):

wherein A¹ and A² are independently hydrogen or C₁-C₅ alkyl. If the final product cannot be obtained as crystals having good filtration properties by ordinary treatments, a novel technique as disclosed herein can provide such crystals by dissolving the reaction product in an organic solvent insoluble or slightly soluble in water; pouring the resultant solution into water; and removing the organic solvent by distillation with stirring to effect the crystallization of the final product.
摘要翻译：公开了通式（2）的2-氰基-4-氧代-4H-苯并吡喃化合物的制备方法：其中R 1和R 2独立地是氢，卤素，羟基，C 1 C 1 -C 20烷氧基，硝基或其中R是C 1 -C 20烷基，苯基，苯基取代的（C 1 -C 20）烷基，苯基（C 1 -C 20）烷氧基苯基或（C 1 -C 20）烷氧基苯基。该制备方法的特征在于通式（1）的羧酰胺：其中R 1和R 2各自如上所定义，其中R 1和R 2分别与脱水剂在吡啶化合物通式（4）：其中A 1和A 2独立地是氢或C 1 -C 5烷基。如果通过常规处理不能获得具有良好过滤性能的结晶的最终产品，则本文公开的新技术可以通过将反应产物溶解在不溶于或微溶于水的有机溶剂中来提供这种晶体; 将所得溶液倒入水中; 并在搅拌下通过蒸馏除去有机溶剂以实现最终产物的结晶。

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