Keisuke Suzuki*, Tomokazu Ogura*, Masaki Hayashi and Tsuyoshi Ueda,
{"title":"建立一种简单有效的非对映体盐结晶光学分辨筛选方案:分析成功的相关因素并从以往研究中构建可靠的程序","authors":"Keisuke Suzuki*, Tomokazu Ogura*, Masaki Hayashi and Tsuyoshi Ueda, ","doi":"10.1021/acs.oprd.5c00201","DOIUrl":null,"url":null,"abstract":"<p >This paper presents a simple and efficient screening protocol for optical resolution by diastereomeric salt crystallization, developed from an analysis of our historical data. Original screening kits have been created utilizing selected commercially available chiral acids and bases, which encompass all reagents that have demonstrated promising results in the diastereomeric salt crystallization of 30 intermediates examined in our laboratories. The influence of various conditions such as crystallization solvents, the equivalents of the resolving agent, additives, and temperature was analyzed to establish clear procedures for the first screening experiments. The advantages of this procedure include its simplicity, accessibility, and high likelihood of success supported by historical achievements, as demonstrated in the optical resolution of the PTDSS1 inhibitor’s intermediate. Overall, this research offers valuable insights into the techniques of diastereomeric salt crystallization and contributes to the efficient acquisition of chiral compounds and advancement of process chemistry.</p>","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":"29 8","pages":"2097–2106"},"PeriodicalIF":3.5000,"publicationDate":"2025-07-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Establishment of a Simple and Efficient Screening Protocol for Optical Resolution by Diastereomeric Salt Crystallization: Analyzing Success-Related Factors and Constructing Reliable Procedures from Previous Studies\",\"authors\":\"Keisuke Suzuki*, Tomokazu Ogura*, Masaki Hayashi and Tsuyoshi Ueda, \",\"doi\":\"10.1021/acs.oprd.5c00201\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >This paper presents a simple and efficient screening protocol for optical resolution by diastereomeric salt crystallization, developed from an analysis of our historical data. Original screening kits have been created utilizing selected commercially available chiral acids and bases, which encompass all reagents that have demonstrated promising results in the diastereomeric salt crystallization of 30 intermediates examined in our laboratories. The influence of various conditions such as crystallization solvents, the equivalents of the resolving agent, additives, and temperature was analyzed to establish clear procedures for the first screening experiments. The advantages of this procedure include its simplicity, accessibility, and high likelihood of success supported by historical achievements, as demonstrated in the optical resolution of the PTDSS1 inhibitor’s intermediate. Overall, this research offers valuable insights into the techniques of diastereomeric salt crystallization and contributes to the efficient acquisition of chiral compounds and advancement of process chemistry.</p>\",\"PeriodicalId\":55,\"journal\":{\"name\":\"Organic Process Research & Development\",\"volume\":\"29 8\",\"pages\":\"2097–2106\"},\"PeriodicalIF\":3.5000,\"publicationDate\":\"2025-07-25\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Organic Process Research & Development\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acs.oprd.5c00201\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, APPLIED\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Organic Process Research & Development","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acs.oprd.5c00201","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
Establishment of a Simple and Efficient Screening Protocol for Optical Resolution by Diastereomeric Salt Crystallization: Analyzing Success-Related Factors and Constructing Reliable Procedures from Previous Studies
This paper presents a simple and efficient screening protocol for optical resolution by diastereomeric salt crystallization, developed from an analysis of our historical data. Original screening kits have been created utilizing selected commercially available chiral acids and bases, which encompass all reagents that have demonstrated promising results in the diastereomeric salt crystallization of 30 intermediates examined in our laboratories. The influence of various conditions such as crystallization solvents, the equivalents of the resolving agent, additives, and temperature was analyzed to establish clear procedures for the first screening experiments. The advantages of this procedure include its simplicity, accessibility, and high likelihood of success supported by historical achievements, as demonstrated in the optical resolution of the PTDSS1 inhibitor’s intermediate. Overall, this research offers valuable insights into the techniques of diastereomeric salt crystallization and contributes to the efficient acquisition of chiral compounds and advancement of process chemistry.
期刊介绍:
The journal Organic Process Research & Development serves as a communication tool between industrial chemists and chemists working in universities and research institutes. As such, it reports original work from the broad field of industrial process chemistry but also presents academic results that are relevant, or potentially relevant, to industrial applications. Process chemistry is the science that enables the safe, environmentally benign and ultimately economical manufacturing of organic compounds that are required in larger amounts to help address the needs of society. Consequently, the Journal encompasses every aspect of organic chemistry, including all aspects of catalysis, synthetic methodology development and synthetic strategy exploration, but also includes aspects from analytical and solid-state chemistry and chemical engineering, such as work-up tools,process safety, or flow-chemistry. The goal of development and optimization of chemical reactions and processes is their transfer to a larger scale; original work describing such studies and the actual implementation on scale is highly relevant to the journal. However, studies on new developments from either industry, research institutes or academia that have not yet been demonstrated on scale, but where an industrial utility can be expected and where the study has addressed important prerequisites for a scale-up and has given confidence into the reliability and practicality of the chemistry, also serve the mission of OPR&D as a communication tool between the different contributors to the field.