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    • 1. 发明申请
    • PROCESS FOR THE PREPARATION OF 1-ALKOXY-1-TRIMETHYLSILYLOXYCYCLOPROPANES
    • 1-烷基-1-三甲氧基硅烷氧基化合物的制备方法
    • WO1998028309A1
    • 1998-07-02
    • PCT/JP1997004705
    • 1997-12-19
    • IHARA CHEMICAL INDUSTRY CO., LTD.YOSHIDA, Yasuo
    • IHARA CHEMICAL INDUSTRY CO., LTD.
    • C07F07/18
    • C07F7/188
    • A process for the preparation of 1-alkoxy-1-trimethylsilyloxycyclopropanes of general formula (I), wherein R and R are each independently hydrogen or lower alkyl; and R is lower alkyl, by reacting finely divided metallic sodium dispersed in a hydrocarbon with a beta -halogeno carboxylic ester of general formula (II), wherein R , R and R are each as defined above; and X is halogen and chlorotrimethylsilane. According to this process, 1-alkoxy-1-trimethylsilyloxypropanes can be industrially prepared, easily, simply and economically advantageously without any special equipment by using not an ethereal solvent problematic in safety but finely divided metallic sodium dispersed in a hydrocarbon in a yield equivalent to or higher than that attained by using an ethereal solvent.
    • 制备通式(I)的1-烷氧基-1-三甲基甲硅烷氧基环丙烷的方法,其中R 1和R 2各自独立地为氢或低级烷基; 和R 3是低级烷基,通过使分散在烃中的细碎金属钠与通式(II)的β-卤代羧酸酯反应,其中R 1,R 2和R 3各自为 如上所述; X为卤素和氯代三甲基硅烷。 根据该方法,1-烷氧基-1-三甲基甲硅烷氧基丙烷可以在工业上制备,容易,简单和经济上有利地没有任何特殊的设备,通过使用不是安全的醚溶剂,而是分散在烃中的细分散的金属钠,产率相当于 或高于通过使用醚类溶剂获得的浓度。
    • 3. 发明申请
    • PROCESSES FOR PRODUCING THIOARYL COMPOUND
    • 生产硫酸化合物的方法
    • WO1995025089A1
    • 1995-09-21
    • PCT/JP1995000455
    • 1995-03-17
    • IHARA CHEMICAL INDUSTRY CO., LTD.SUGIYAMA, TatsuoNAKAYAMA, Tadashi
    • IHARA CHEMICAL INDUSTRY CO., LTD.
    • C07C319/06
    • C07C319/14C07C319/06C07C323/52C07C323/34
    • A process for producing an alkali metal salt of an arylmercaptan compound represented by general formula (3), by the reaction of a disulfide compound represented by general formula (1) with a hydroxide of an alkali metal M in the presence of a sulfur compound represented by the general formula (2): H(2-i)S(M )i, another process for producing an alkoxycarbonylalkylthioaryl compound represented by general formula (5) by the reaction of the alkali metal salt of an arylmercaptan compound obtained above with a halogenated fatty acid ester represented by the general formula (4): X -R -COOR at a pH of 7 to 10; and still another process for producing the alkoxycarbonylalkylthioaryl compound by the reaction of the disulfide compound with the hydroxide of an alkali metal M in the presence of the sulfur compound, followed by the reaction of the obtained alkali metal salt of an arylmercaptan compound, without being isolated, with the halogenated fatty acid ester under the same condition.
    • 一种通式(3)表示的芳基硫醇化合物的碱金属盐的制备方法,通过在通式(1)表示的二硫化物与碱金属M 1的氢氧化物的反应中, 由通式(2)表示的硫化合物:H(2-i)S(M 1)i,另外通过通式(5)表示的烷氧基羰基烷基硫代芳基化合物的制备方法, 在通式(4)表示的卤代脂肪酸酯:X 1 -R 2 -COOR 3,pH7〜10的条件下,得到上述得到的芳基硫醇化合物; 还有在硫化合物存在下,通过二硫化物与碱金属M 1的氢氧化物的反应制备烷氧基羰基烷基硫代芳基化合物的另一种方法,然后将所得到的芳基硫醇化合物的碱金属盐, 在不同的条件下与卤代脂肪酸酯分离。
    • 4. 发明申请
    • PROCESS FOR PRODUCING HEXAHYDROPYRIDAZINE AND HEXAHYDROPYRIDAZINE-1,2-DICARBOXYLATE DERIVATIVE
    • 六氢呋喃并嘧啶衍生物的制造方法和二氢吡啶-2-基二甲氧基硅烷衍生物
    • WO1995021828A1
    • 1995-08-17
    • PCT/JP1995000184
    • 1995-02-10
    • IHARA CHEMICAL INDUSTRY CO., LTD.SUGIYAMA, Tatsuo
    • IHARA CHEMICAL INDUSTRY CO., LTD.
    • C07D237/04
    • C07D237/04
    • A process for producing a hexahydropyridazine-1,2-dicarboxylate derivative represented by general formula (3) (wherein R and R represent each independently alkyl) by reacting a hydrazinedicarboxylate derivative represented by the general formula (1): R OOC-NH-NH-COOR (wherein R and R are each as defined above) with a dihalogenobutane represented by the general formula (2): X -CH2CH2CH2CH2-X (wherein X and X represent each independently halogen) in the presence of an alkali metal hydroxide, characterized by conducting the reaction in an aprotic polar solvent; and a process for producing hexahydropyridazine by decarboxylating the obtained hexahydropyridazine-1,2-dicarboxylate derivative (3), without being isolated, in the presence of an alkali metal hydroxide and a hydrogen donor compound.
    • 由通式(3)表示的肼基二羧酸酯衍生物(1)表示的通式(3)表示的六氢哒嗪-1,2-二羧酸酯衍生物的制造方法(其中R 1和R 2各自独立地为烷基) R 2 OOC-NH-NH-COOR 2(其中R 1和R 2各自如上所定义)与通式(2)表示的二卤代丁烷:X 1 -CH 2 CH 2 CH 2 CH 2 - X 2(其中X 1和X 2各自独立地为卤素)在碱金属氢氧化物的存在下反应,其特征在于在非质子极性溶剂中进行反应; 以及通过在碱金属氢氧化物和氢供体化合物的存在下将所得六氢哒嗪-1,2-二羧酸酯衍生物(3)脱羧而不分离来制备六氢哒嗪的方法。
    • 10. 发明申请
    • PROCESS FOR PRODUCING 2-SUBSTITUTED BENZO[b]THIOPHENE
    • 生产2-取代苯并[b]噻吩的方法
    • WO1995009165A1
    • 1995-04-06
    • PCT/JP1994001578
    • 1994-09-26
    • IHARA CHEMICAL INDUSTRY CO., LTD.YAZAWA, NaotoSAITO, YoshinoriHIYOSHI, HidetakaYOSHIDA, Yasuo
    • IHARA CHEMICAL INDUSTRY CO., LTD.
    • C07D333/56
    • C07D333/60C07D333/56C07D333/70
    • An industrial process for producing a 2-substituted benzo[b]thiophene which is highly effective in that it can afford the target compound in a high yield with a simple operation without the necessity for using unstable starting materials. The process comprises reacting an optionally substituted 2-halogenobenzaldehyde with either a compound represented by the general formula (1): HiSjMk (wherein M represents an alkali metal atom; i represents an integer of 0 or 1; j represents an integer of 1 or above; and k represents an integer of 1 or 2; provided i + k = 2) and sulfur, or a compound represented by the above formula (1) (wherein j is 2 or above) in the presence of an aprotic polar solvent, and then reacting the reaction product with a compound represented by the general formula (2): XCH2R (wherein X represents a halogen atom; and R represents acyl, optionally substituted alkoxycarbonyl, optionally substituted arylcarbonyl, or cyano) to effect intramolecular ring closure.
    • 用于生产2-取代的苯并[b]噻吩的工业方法是非常有效的,因为它可以通过简单的操作以高产率获得目标化合物,而不需要使用不稳定的起始材料。 该方法包括使任选取代的2-卤代苯甲醛与由通式(1)表示的化合物:HiSjMk(其中M表示碱金属原子; i表示0或1的整数; j表示1以上的整数) ; k表示1或2的整数; i + k = 2)和硫,或由上式(1)表示的化合物(其中j为2以上)在非质子极性溶剂的存在下,以及 然后使反应产物与由通式(2)表示的化合物:XCH 2 R(其中X表示卤素原子; R表示酰基,任选取代的烷氧基羰基,任选取代的芳基羰基或氰基)反应以实现分子内闭环。