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    • 3. 发明申请
    • METHOD OF PREPARING 10H-DIBENZO[b,f]]1,4]THIAZEPIN-11-ONE
    • 制备10H-二苯并[b,f]] 1,4]噻吩并-11-酮的方法
    • WO2004047722A2
    • 2004-06-10
    • PCT/KR0302579
    • 2003-11-26
    • SK CORPKWAK BYONG-SUNGCHUNG KI-NAMKOH KI-HOHWANG HEE-JUN
    • KWAK BYONG-SUNGCHUNG KI-NAMKOH KI-HOHWANG HEE-JUN
    • C07D281/16A61K
    • C07D281/16
    • Disclosed is a method of preparing 10H-dibenzo[b,f][1,4]thiazepin-11-one, including reacting dithiosalicylic acid with 1-chloro-2-nitrobenzene in a basic aqueous solution in the presence of absence of a reducing agent, to prepare 2-(2-nitrophenylsulfuryl)benzoic acid; subjecting the 2-(2-nitrophenylsulfuryl)benzoic acid to nitro group reduction in the presence of hydrogen, a solvent and a heterogeneous metal catalyst, to prepare 2-(2-aminophenylsulfuryl)benzoic acid; and directly cyclizing the 2-(2-aminophenylsulfuryl)benzoic acid in an organic solvent in the presence or absence of an acid catalyst. The method according to the present invention is economical due to the use of the inexpensive starting material, and also environmentally friendly and efficient by minimizing the use of the organic solvent and performing direct cyclization without the activation of carboxylic acid.
    • 公开了一种制备10H-二苯并[b,f] [1,4]硫杂吖庚因-11-酮的方法,包括在碱性水溶液中,在不存在还原剂的情况下,将二硫代水杨酸与1-氯-2-硝基苯反应 制备2-(2-硝基苯基硫基)苯甲酸; 在氢气,溶剂和非均相金属催化剂的存在下使2-(2-硝基苯基亚磺酰基)苯甲酸进行硝基还原,制备2-(2-氨基苯基硫基)苯甲酸; 并在酸催化剂存在或不存在下,在有机溶剂中直接环化2-(2-氨基苯基硫基)苯甲酸。 根据本发明的方法由于使用廉价的起始材料而是经济的,并且通过最小化有机溶剂的使用并且在没有羧酸活化的情况下进行直接环化,也是环境友好和有效的。
    • 6. 发明申请
    • PROCESS FOR THE PREPARATION OF 11-(4-[2-(2-HYDROXYETHOXY)ETHYL]-I-PIPERAZINYL)DIB ENZO[b,f][l,4]THIAZEPINE
    • 制备11-(4- [2-(2-羟基乙氧基)乙基] -1-哌啶子基)DIB ENZO [b,f] [1,4]噻唑的方法
    • WO2006001619A1
    • 2006-01-05
    • PCT/KR2005/001866
    • 2005-06-17
    • SK CORPORATIONKWAK, Byong, SungLEE, Sang, IlHWANG, Hee, JunLIM, Jong, Ho
    • KWAK, Byong, SungLEE, Sang, IlHWANG, Hee, JunLIM, Jong, Ho
    • C07D417/04
    • C07D281/16
    • Disclosed is a process for the preparation of l l-(4-[2-(2-hydroxyethoxy)ethyl]-l- piperazinyl)-dibenzo[b,f][l,4]thiazepine. In the process, low-priced 2,2'-dithiosalicylic acid as starting material is subjected to bond formation reaction with l-chloro-2- 5 nitrobenzene in a basic aqueous solution, a nitro group reduction reaction is conducted, cyclization and chlorination reactions are simultaneously carried out in the presence of a equivalent amount of halogenating agent, a reaction with piperazine is continuously conducted without separation, and a reaction with 2-haloethoxyethanol is conducted, thereby it is possible to economically producing Quetiapine, that is, l l-(4-[2-(2- 10 hydroxyethoxy)ethyl]-l-piperazinyl)-dibenzo[b,fj[l,4]thiazepine, in an environmentally friendly manner. Particularly, the process is advantageous in that economic efficiency is assured because of use of the low-priced starting material, use of an organic solvent is minimized because a reaction is conducted in an aqueous solution, and it is possible to achieve the environmentally friendly and economical process having high commercial 15 usefulness because the number of reaction steps of the process is reduced and because generation of acidic waste is minimized.
    • 公开了制备11-(4- [2-(2-羟基乙氧基)乙基] -1-哌嗪基) - 二苯并[b,f] [1,4]硫杂吖庚因的方法。 在此过程中,作为起始原料的低价2,2'-二硫代水杨酸与碱性水溶液中的1-氯-2-硝基苯进行结合形成反应,进行硝基还原反应,进行环化和氯化反应 在等量的卤化剂的存在下同时进行,与哌嗪的反应在不分离的条件下连续进行,与2-卤代乙氧基乙醇进行反应,从而可以经济地制备喹硫平,即, (4- [2-(2-10羟基乙氧基)乙基] -1-哌嗪基) - 二苯并[b,f] [1,4]硫氮杂。 特别地,该方法的优点在于,由于使用低价起始材料来确保经济效率,因此在水溶液中进行反应而使有机溶剂的使用最小化,并且可以实现环境友好和 因为该方法的反应步骤数量减少并且由于酸性废物的产生被最小化而具有高商业性的有用性的经济方法。