公开(公告)号：US08809486B2

公开(公告)日：2014-08-19

申请号：US13548934

申请日：2012-07-13

申请人： Venkata Rama Narayanan Ganapathy Bhotla ,  Balakrishnan Ganesan ,  Kishan Gurram ,  Salkod Parameshwar Mallika ,  Kumar Arun Satyanarayana ,  Swaminathan Shubashree

发明人： Venkata Rama Narayanan Ganapathy Bhotla ,  Balakrishnan Ganesan ,  Kishan Gurram ,  Salkod Parameshwar Mallika ,  Kumar Arun Satyanarayana ,  Swaminathan Shubashree

IPC分类号： C08G73/10 ,  C08G73/00 ,  C08G73/06

CPC分类号： C07D209/46 ,  C08G64/12

摘要： Disclosed is a method for producing a purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I) wherein R1 is hydrogen or a C1-25 hydrocarbyl group and R2 is a hydrogen, a C1-25 hydrocarbyl group, or a halogen, and wherein the method comprises dissolving a crude phthalimidine compound in an aqueous base solution; precipitating the dissolved, crude phthalimidine compound from the aqueous base solution by adding an acid in an amount effective to lower the pH of the solution to 9.0 to 12.0, to provide a semicrude phthalimidine compound; and isolating the semicrude phthalimidine compound from the aqueous base solution, to provide the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I), and having a phenolphthalein compound content of less than 2,500 ppm, based on the weight of the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine. Subsequent trituration with aqueous methanol and recrystallization from isopropanol can result in product having undetectable levels of phenolphthalein derivatives.

摘要翻译： 公开了一种制备式（I）的纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶的方法，其中R1是氢或C1-25烃基，R2是氢，C1-25烃基 基团或卤素，并且其中所述方法包括将粗的邻苯二酰亚胺化合物溶解在碱性水溶液中; 通过加入一种有效降低溶液pH至9.0至12.0的酸，从碱性水溶液中沉淀出溶解的粗的苯并二氮嘧啶化合物，得到半羟基苯并二氮嘧啶化合物; 并从碱水溶液中分离半代邻苯二甲酰亚胺化合物，得到纯化的式（I）2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶，其酚酞化合物含量小于2,500ppm，基于 关于纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮吡啶的重量。 随后用甲醇水溶液研磨并从异丙醇中重结晶可导致具有不可检测水平的酚酞衍生物的产物。

公开(公告)号：US07790832B2

公开(公告)日：2010-09-07

申请号：US11849523

申请日：2007-09-04

申请人： Balakrishnan Ganesan ,  Pradeep Jeevaji Nadkarni ,  Kumar Arun Satyanarayana ,  Venkata Rama Narayanan Ganapathy Bhotla ,  Suresh Shanumgam ,  Gurram Kishan ,  Ravindra Vikram Singh

发明人： Balakrishnan Ganesan ,  Pradeep Jeevaji Nadkarni ,  Kumar Arun Satyanarayana ,  Venkata Rama Narayanan Ganapathy Bhotla ,  Suresh Shanumgam ,  Gurram Kishan ,  Ravindra Vikram Singh

IPC分类号： C08G64/00 ,  C08G63/02

CPC分类号： C07D209/46 ,  C08G64/12

摘要： A method for purifying a 2-aryl-3,3-bis(hydroxyaryl)phthalimidine comprises contacting a crude 2-aryl-3,3-bis(hydroxyaryl)phthalimidine with a purification agent, removing a 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound from the crude 2-aryl-3,3-bis(hydroxyaryl)phthalimidine, and producing a purified 2-aryl-3,3-bis(hydroxyaryl)phthalimidine product comprising less than 200 parts per million of the 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound. The purification agent is selected from the group consisting of an acidic material, an organic acid chloride, an organic anhydride, or a combination thereof. The 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound has a formula: wherein each R1 is independently selected from a group consisting of a hydrocarbyl radical, a nitro radical, and a halogen atom; “a” is an integer from 0 to 4; and Ar1 and Ar2 are independently at each occurrence an aromatic radical. The purified 2-aryl-3,3-bis(hydroxyaryl)phthalimidines have low color, and are useful for preparing polymers, such as polycarbonates having a low color. The polycarbonates are useful for producing articles.

摘要翻译： 纯化2-芳基-3,3-双（羟基芳基）苯并二氮嘧啶的方法包括使粗2-二芳基-3,3-双（羟基芳基）苯并二氮吡啶与纯化剂接触，除去2-芳基-3-（氨基芳基 ）-3-（羟基芳基）苯并二氮嘧啶化合物，并制备纯化的2-芳基-3,3-双（羟基芳基）苯并二氮嘧啶产物，其包含小于200份 百万的2-芳基-3-（氨基芳基）-3-（羟基芳基）苯并嘧啶化合物。 净化剂选自酸性物质，有机酰氯，有机酸酐或其组合。 2-芳基-3-（氨基芳基）-3-（羟基芳基）苯并二氮嘧啶化合物具有下式：其中每个R 1独立地选自烃基，硝基和卤素原子; “a”是从0到4的整数; Ar 1和Ar 2在每次出现时独立地为芳族基团。 纯化的2-芳基-3,3-双（羟基芳基）苯二甲酰亚胺具有低的颜色，并且可用于制备聚合物，例如具有低颜色的聚碳酸酯。 聚碳酸酯可用于制造制品。

公开(公告)号：US20100152416A1

公开(公告)日：2010-06-17

申请号：US12333451

申请日：2008-12-12

申请人： Venkata Rama Narayanan Ganapathy BHOTLA ,  Balakrishnan GANESAN ,  Kishan Gurram ,  Salkod Parameshwar MALLIKA ,  Kumar Arun Satyanarayana ,  Swaminathan SHUBASHREE

发明人： Venkata Rama Narayanan Ganapathy BHOTLA ,  Balakrishnan GANESAN ,  Kishan Gurram ,  Salkod Parameshwar MALLIKA ,  Kumar Arun Satyanarayana ,  Swaminathan SHUBASHREE

IPC分类号： C08G73/06 ,  C07D209/48 ,  C07D307/20

CPC分类号： C07D209/46 ,  C08G64/12

摘要： Disclosed herein is a method for producing a purified 2-aryl-3,3-bis(4-hydroxyaryl) phthalimidine of formula (I) wherein R1 is hydrogen or a C1-25 hydrocarbyl group and R2 is a hydrogen, a C1-25 hydrocarbyl group, or a halogen, and wherein the method comprises dissolving a crude phthalimidine compound in an aqueous base solution; precipitating the dissolved, crude phthalimidine compound from the aqueous base solution by adding an acid in an amount effective to lower the pH of the solution to 9.0 to 12.0, to provide a semicrude phthalimidine compound; and isolating the semicrude phthalimidine compound from the aqueous base solution, to provide the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I), and having a phenolphthalein compound content of less than 2,500 ppm, based on the weight of the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine. Subsequent trituration with aqueous methanol and recrystallization from isopropanol can result in product having levels of phenolphthalein derivatives that are not detectable.

摘要翻译： 本文公开了一种制备式（I）的纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶的方法，其中R1是氢或C1-25烃基，R2是氢，C1-25 烃基或卤素，并且其中所述方法包括将粗的邻苯二甲酰亚胺化合物溶解在碱性水溶液中; 通过加入一种有效降低溶液pH至9.0至12.0的酸，从碱性水溶液中沉淀出溶解的粗的苯并二氮嘧啶化合物，得到半羟基苯并二氮嘧啶化合物; 并从碱水溶液中分离半代邻苯二甲酰亚胺化合物，得到纯化的式（I）2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶，其酚酞化合物含量小于2,500ppm，基于 关于纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮吡啶的重量。 随后用甲醇水溶液研磨并从异丙醇中重结晶可产生具有不可检测的酚酞衍生物含量的产物。

公开(公告)号：US20120309926A1

公开(公告)日：2012-12-06

申请号：US13548934

申请日：2012-07-13

申请人： Venkata Rama Narayanan Ganapathy BHOTLA ,  Balakrishnan GANESAN ,  Kishan GURRAM ,  Salkod Parameshwar MALLIKA ,  Kumar Arun SATYANARAYANA ,  Swaminathan SHUBASHREE

发明人： Venkata Rama Narayanan Ganapathy BHOTLA ,  Balakrishnan GANESAN ,  Kishan GURRAM ,  Salkod Parameshwar MALLIKA ,  Kumar Arun SATYANARAYANA ,  Swaminathan SHUBASHREE

IPC分类号： C07D209/46 ,  C08G73/06

CPC分类号： C07D209/46 ,  C08G64/12

摘要： Disclosed is a method for producing a purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I) wherein R1 is hydrogen or a C1-25 hydrocarbyl group and R2 is a hydrogen, a C1-25 hydrocarbyl group, or a halogen, and wherein the method comprises dissolving a crude phthalimidine compound in an aqueous base solution; precipitating the dissolved, crude phthalimidine compound from the aqueous base solution by adding an acid in an amount effective to lower the pH of the solution to 9.0 to 12.0, to provide a semicrude phthalimidine compound; and isolating the semicrude phthalimidine compound from the aqueous base solution, to provide the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I), and having a phenolphthalein compound content of less than 2,500 ppm, based on the weight of the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine. Subsequent trituration with aqueous methanol and recrystallization from isopropanol can result in product having undetectable levels of phenolphthalein derivatives.

摘要翻译： 公开了一种制备式（I）的纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶的方法，其中R1是氢或C1-25烃基，R2是氢，C1-25烃基 基团或卤素，并且其中所述方法包括将粗的邻苯二酰亚胺化合物溶解在碱性水溶液中; 通过加入一种有效降低溶液pH至9.0至12.0的酸，从碱性水溶液中沉淀出溶解的粗的苯并二氮嘧啶化合物，得到半羟基苯并二氮嘧啶化合物; 并从碱水溶液中分离半代邻苯二甲酰亚胺化合物，得到纯化的式（I）2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶，其酚酞化合物含量小于2,500ppm，基于 关于纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮吡啶的重量。 随后用甲醇水溶液研磨并从异丙醇中重结晶可导致具有不可检测水平的酚酞衍生物的产物。

公开(公告)号：US07563817B2

公开(公告)日：2009-07-21

申请号：US11300225

申请日：2005-12-14

申请人： Balakrishnan Ganesan ,  Pradeep Jeevaji Nadkarni ,  Kumar Arun Satyanarayana ,  Venkata Rama Narayanan Ganapathy Bhotla ,  Suresh Shanmugam ,  Gurram Kishan ,  Ravindra Vikram Singh

发明人： Balakrishnan Ganesan ,  Pradeep Jeevaji Nadkarni ,  Kumar Arun Satyanarayana ,  Venkata Rama Narayanan Ganapathy Bhotla ,  Suresh Shanmugam ,  Gurram Kishan ,  Ravindra Vikram Singh

IPC分类号： A61K31/405 ,  C07D209/34

CPC分类号： C07D209/46 ,  C08G64/12

摘要： A method for purifying a 2-aryl-3,3-bis(hydroxyaryl)phthalimidine comprises contacting a crude 2-aryl-3,3-bis(hydroxyaryl)phthalimidine with a purification agent, removing a 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound from the crude 2-aryl-3,3-bis(hydroxyaryl)phthalimidine, and producing a purified 2-aryl-3,3-bis(hydroxyaryl)phthalimidine product comprising less than 200 parts per million of the 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound. The purification agent is selected from the group consisting of an acidic material, an organic acid chloride, an organic anhydride, or a combination thereof. The 2-aryl-3-(aminoaryl)-3-(hydroxyaryl)phthalimidine compound has a formula: wherein each R1 is independently selected from a group consisting of a hydrocarbyl radical, a nitro radical, and a halogen atom; “a” is an integer from 0 to 4; and Ar1 and Ar2 are independently at each occurrence an aromatic radical. The purified 2-aryl-3,3-bis(hydroxyaryl)phthalimidines have low color, and are useful for preparing polymers, such as polycarbonates having a low color. The polycarbonates are useful for producing articles.

摘要翻译： 纯化2-芳基-3,3-双（羟基芳基）苯并二氮嘧啶的方法包括使粗2-二芳基-3,3-双（羟基芳基）苯并二氮吡啶与纯化剂接触，除去2-芳基-3-（氨基芳基 ）-3-（羟基芳基）苯并二氮嘧啶化合物，并制备纯化的2-芳基-3,3-双（羟基芳基）苯并二氮嘧啶产物，其包含小于200份 百万的2-芳基-3-（氨基芳基）-3-（羟基芳基）苯并嘧啶化合物。 净化剂选自酸性物质，有机酰氯，有机酸酐或其组合。 2-芳基-3-（氨基芳基）-3-（羟基芳基）苯并二氮嘧啶化合物具有下式：其中每个R 1独立地选自烃基，硝基和卤素原子; “a”是从0到4的整数; Ar 1和Ar 2在每次出现时独立地为芳族基团。 纯化的2-芳基-3,3-双（羟基芳基）苯二甲酰亚胺具有低的颜色，并且可用于制备聚合物，例如具有低颜色的聚碳酸酯。 聚碳酸酯可用于制造制品。

公开(公告)号：US08247523B2

公开(公告)日：2012-08-21

申请号：US12333451

申请日：2008-12-12

申请人： Venkata Rama Narayanan Ganapathy Bhotla ,  Balakrishnan Ganesan ,  Kishan Gurram ,  Salkod Parameshwar Mallika ,  Kumar Arun Satyanarayana ,  Swaminathan Shubashree

发明人： Venkata Rama Narayanan Ganapathy Bhotla ,  Balakrishnan Ganesan ,  Kishan Gurram ,  Salkod Parameshwar Mallika ,  Kumar Arun Satyanarayana ,  Swaminathan Shubashree

IPC分类号： C08G73/10 ,  C08G73/00 ,  C08G73/06

CPC分类号： C07D209/46 ,  C08G64/12

摘要： Disclosed herein is a method for producing a purified 2-aryl-3,3-bis(4-hydroxyaryl) phthalimidine of formula (I) wherein R1 is hydrogen or a C1-25 hydrocarbyl group and R2 is a hydrogen, a C1-25 hydrocarbyl group, or a halogen, and wherein the method comprises dissolving a crude phthalimidine compound in an aqueous base solution; precipitating the dissolved, crude phthalimidine compound from the aqueous base solution by adding an acid in an amount effective to lower the pH of the solution to 9.0 to 12.0, to provide a semicrude phthalimidine compound; and isolating the semicrude phthalimidine compound from the aqueous base solution, to provide the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine of formula (I), and having a phenolphthalein compound content of less than 2,500 ppm, based on the weight of the purified 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidine. Subsequent trituration with aqueous methanol and recrystallization from isopropanol can result in product having levels of phenolphthalein derivatives that are not detectable.

摘要翻译： 本文公开了一种制备式（I）的纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶的方法，其中R1是氢或C1-25烃基，R2是氢，C1-25 烃基或卤素，并且其中所述方法包括将粗的邻苯二甲酰亚胺化合物溶解在碱性水溶液中; 通过加入一种有效降低溶液pH至9.0至12.0的酸，从碱性水溶液中沉淀出溶解的粗的苯并二氮嘧啶化合物，得到半羟基苯并二氮嘧啶化合物; 并从碱水溶液中分离半代邻苯二甲酰亚胺化合物，得到纯化的式（I）2-芳基-3,3-双（4-羟基芳基）苯并二氮嘧啶，其酚酞化合物含量小于2,500ppm，基于 关于纯化的2-芳基-3,3-双（4-羟基芳基）苯并二氮吡啶的重量。 随后用甲醇水溶液研磨并从异丙醇中重结晶可产生具有不可检测的酚酞衍生物含量的产物。