公开(公告)号：US07777056B2

公开(公告)日：2010-08-17

申请号：US11547533

申请日：2004-03-30

申请人： Milind Moreshwar Gharpure ,  Swapnil Panditrao Sonawane ,  Srihari Shivaji Mane ,  Rajendra Dagesing Mahale

发明人： Milind Moreshwar Gharpure ,  Swapnil Panditrao Sonawane ,  Srihari Shivaji Mane ,  Rajendra Dagesing Mahale

IPC分类号： C07D311/02

CPC分类号： C07D309/30

摘要： A process for preparation of 4-hydroxy-pyran-2-one derivative of formula (I), wherein R is, and wherein R1 and R2 are methyl and R3 is hydrogen or methyl, comprising the steps of, heating a compound of formula (II), wherein R is as defined before, and R4 is hydrogen, NH4+ or an alkali metal, in a solvent mixture consisting of an aromatic hydrocarbon and a ketone in an inert atmosphere at a temperature of between 60° C. to 92° C. in the absence or presence of orthophosphoric acid or its alkali dihydrogen salts or alkali hydrogen salts of a dibasic acid, followed by optional neutralization of the reaction mixture with an organic base and obtaining compound of formula (I) in high purity and substantially free of impurities through a step of isolation and crystallization. The process leads to formation of derivatives of formula I in high purity with dimmer impurity (III) less than 0.1% and anhydro impurity (IV) below 0.15%.

摘要翻译： 一种制备式（I）的4-羟基 - 吡喃-2-酮衍生物的方法，其中R为，并且其中R 1和R 2为甲基且R 3为氢或甲基，包括以下步骤：加热式 II），其中R如前所定义，并且R 4是氢，NH 4 +或碱金属，在惰性气氛中，在60℃至92℃的温度下在由芳族烃和酮组成的溶剂混合物中 在不存在或存在正磷酸或其二氢酸的碱式二氢盐或碱式氢盐的情况下，随后将有机碱任选地中和反应混合物，得到高纯度且基本上不含 杂质通过分离和结晶的步骤。 该方法导致以高纯度形成式I的衍生物，其中较少的杂质（III）小于0.1％，而脱水杂质（IV）低于0.15％。

公开(公告)号：US20080269508A1

公开(公告)日：2008-10-30

申请号：US11547533

申请日：2004-03-30

申请人： Milind Moreshwar Gharpure ,  Swapnil Panditrao Sonawane ,  Srihari Shivaji Mane ,  Rajendra Dagesing Mahale

发明人： Milind Moreshwar Gharpure ,  Swapnil Panditrao Sonawane ,  Srihari Shivaji Mane ,  Rajendra Dagesing Mahale

IPC分类号： C07D309/30

CPC分类号： C07D309/30

摘要： A process for preparation of 4-hydroxy-pyran-2-one derivative of formula (I), wherein R is, and wherein R1 and R2 are methyl and R3 is hydrogen or methyl, comprising the steps of, heating a compound of formula (II), wherein R is as defined before, and R4 is hydrogen, NH4+ or an alkali metal, in a solvent mixture consisting of an aromatic hydrocarbon and a ketone in an inert atmosphere at a temperature of between 60° C. to 92° C. in the absence or presence of orthophosphoric acid or its alkali dihydrogen salts or alkali hydrogen salts of a dibasic acid, followed by optional neutralization of the reaction mixture with an organic base and obtaining compound of formula (I) in high purity and substantially free of impurities through a step of isolation and crystallization. The process leads to formation of derivatives of formula I in high purity with dimmer impurity (III) less than 0.1% and anhydro impurity (IV) below 0.15%.

摘要翻译： 制备式（I）的4-羟基 - 吡喃-2-酮衍生物的方法，其中R为，并且其中R 1和R 2为甲基，R 包括以下步骤：加热式（II）化合物，其中R如前定义，R 4是氢，NH 3 在惰性气氛中在60℃至92℃的温度下在由芳族烃和酮组成的溶剂混合物中的碱金属或碱金属在 正磷酸或其二元酸的碱式二氢盐或碱式氢盐的存在或不存在，然后任选地用有机碱中和反应混合物，并得到高纯度且基本上不含杂质的式（I）化合物 隔离和结晶的步骤。 该方法导致以高纯度形成式I的衍生物，其中较少的杂质（III）小于0.1％，而脱水杂质（IV）低于0.15％。