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    • 9. 发明公开
    • L-α-글리세로포스포릴 콜린의 제조방법
    • 一种制备L-阿尔法 - 甘油磷酸胆碱的方法
    • KR1020070119176A
    • 2007-12-20
    • KR1020060053441
    • 2006-06-14
    • 주식회사 대웅제약대웅바이오 주식회사
    • 송윤석송은섭강두성송인웅강필구오성수문성철이병구
    • C07F9/10C07F9/02
    • C07F9/091C07F9/113A61K31/6615
    • A process for preparation of L-alpha-glycerophosphoryl choline is provided to reduce preparation costs by using an inexpensive starting material and a small amount of ion exchange resin, improve preparation yield and is applied to the industrial scale. A process for preparation of L-alpha-glycerophosphoryl choline represented by the formula(1) comprises the steps of: removing calcium from compounds represented by the formula(2) under acid condition at -10 to 60 deg.C and pH 2 or less to prepare compounds represented by the formula(3); reacting the compounds represented by the formula(3) with compounds represented by the formula(4) in solvent selected from C1-C6 alcohol, C1-C6 ether, C1-C6 ketone and a mixture thereof at 40-120 deg.C and pH 5-10 to prepare compounds represented by the formula(5); crystallizing the compounds represented by the formula(5) by using a crystallizing agent selected from C1-C6 alcohol, C1-C6 ketone and a mixture thereof at 0-25 deg.C; and subjecting the compounds represented by the formula(5) to ion exchange resin so as to remove chlorine ion.
    • 提供了一种制备L-α-甘油磷酰胆碱的方法,通过使用廉价的原料和少量的离子交换树脂来降低制备成本,提高了制备成品率,并被应用于工业规模。 由式(1)表示的制备L-α-甘油磷酰胆碱的方法包括以下步骤:在酸性条件下在-10至60℃和pH 2或更低的条件下从式(2)表示的化合物中除去钙 制备由式(3)表示的化合物; 使式(3)表示的化合物与式(4)表示的化合物在选自C 1 -C 6醇,C 1 -C 6醚,C 1 -C 6酮及其混合物的溶剂中在40-120摄氏度和pH 5-10制备由式(5)表示的化合物; 在0-25℃使用选自C 1 -C 6醇,C 1 -C 6酮及其混合物的结晶剂使式(5)表示的化合物结晶; 并将式(5)表示的化合物进行离子交换树脂以除去氯离子。
    • 10. 发明公开
    • 란소프라졸 결정형 A의 제조방법
    • 制备兰索唑晶型的方法
    • KR1020070073419A
    • 2007-07-10
    • KR1020060001303
    • 2006-01-05
    • 주식회사 대웅제약대웅바이오 주식회사
    • 문성철송인웅강두성오성수이성재
    • C07D401/12
    • C07D401/12
    • A method for preparing crystalline form A of lasnoprazole is provided to mass-produce the crystalline form A of lasnoprazole with high purity without a separate converting step from an ethanol solvent by adjusting the temperature and agitation time required for crystallization. The method comprises the steps of: (a) after dissolving 1 part by weight of lansoprazole obtained by oxidizing 2-([3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl]-methyl)thio-1H-benzimidazole in 1-50 parts by weight of ethanol, adding water thereto; (b) agitating the product obtained from the step(a) at a temperature of 15-40 deg.C for 0.5-4 hours; and (c) filtering and drying the product obtained from the step(b). Before adding the water, the color of the solution is removed by using charcoal and Na2S2O4.
    • 提供了一种制备拉唑诺唑结晶A的方法,通过调节结晶所需的温度和搅拌时间,大量生产高纯度的拉诺拉唑的结晶形式A,而无需通过乙醇溶剂的单独转化步骤。 该方法包括以下步骤:(a)将1 - ((3-甲基-4-(2,2,2-三氟乙氧基)-2-吡啶基] - 甲基)硫代 - 1-苯并咪唑在1-50重量份乙醇中,向其中加入水; (b)在15-40℃的温度下搅拌从步骤(a)获得的产物0.5-4小时; 和(c)过滤并干燥由步骤(b)获得的产物。 加入水之前,用炭和Na2S2O4去除溶液的颜色。