{"title":"放大微波加速有机合成。","authors":"H Lehmann","doi":"10.1007/2789_2007_032","DOIUrl":null,"url":null,"abstract":"<p><p>Microwave-assisted organic chemistry has received strong exposure in the literature over the last decade, and nowadays more and more research chemists are successfully applying microwave technology to organic reactions on a small scale. However, the efficient application of this technology to cover the specific needs of larger-scale preparations, e.g., in a kilo lab, remains to be shown. We therefore initiated a study to investigate the scalability of microwave technology. Two different microwave systems designed for large-scale operation were evaluated in order to characterize strengths and weaknesses of each instrument with regard to scale-up. Special focus was directed on temperature/pressure limits, handling of suspensions, ability to rapidly heat and cool, robustness, and overall processing time. Based on the results of this study, a batch microwave reactor with a reaction volume of approximately 1.1 1 was purchased and installed in the kilo lab. Several reactions have been performed successfully on a 50- to 100-g scale in our laboratory, showing that a scale-up from a 15 ml scale to a 1-1 scale is feasible. In general, a significant reduction of reaction time was achievable, in some cases yields and selectivity were also improved. Nevertheless, a major weakness of the available systems is the limited vessel size, which is, in most cases, far below a suitable reaction volume required for work in a kilo lab.</p>","PeriodicalId":87471,"journal":{"name":"Ernst Schering Foundation symposium proceedings","volume":" 3","pages":"133-49"},"PeriodicalIF":0.0000,"publicationDate":"2006-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1007/2789_2007_032","citationCount":"6","resultStr":"{\"title\":\"Scale-up in microwave-accelerated organic synthesis.\",\"authors\":\"H Lehmann\",\"doi\":\"10.1007/2789_2007_032\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>Microwave-assisted organic chemistry has received strong exposure in the literature over the last decade, and nowadays more and more research chemists are successfully applying microwave technology to organic reactions on a small scale. However, the efficient application of this technology to cover the specific needs of larger-scale preparations, e.g., in a kilo lab, remains to be shown. We therefore initiated a study to investigate the scalability of microwave technology. Two different microwave systems designed for large-scale operation were evaluated in order to characterize strengths and weaknesses of each instrument with regard to scale-up. Special focus was directed on temperature/pressure limits, handling of suspensions, ability to rapidly heat and cool, robustness, and overall processing time. Based on the results of this study, a batch microwave reactor with a reaction volume of approximately 1.1 1 was purchased and installed in the kilo lab. Several reactions have been performed successfully on a 50- to 100-g scale in our laboratory, showing that a scale-up from a 15 ml scale to a 1-1 scale is feasible. In general, a significant reduction of reaction time was achievable, in some cases yields and selectivity were also improved. Nevertheless, a major weakness of the available systems is the limited vessel size, which is, in most cases, far below a suitable reaction volume required for work in a kilo lab.</p>\",\"PeriodicalId\":87471,\"journal\":{\"name\":\"Ernst Schering Foundation symposium proceedings\",\"volume\":\" 3\",\"pages\":\"133-49\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2006-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.1007/2789_2007_032\",\"citationCount\":\"6\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Ernst Schering Foundation symposium proceedings\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.1007/2789_2007_032\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"\",\"JCRName\":\"\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Ernst Schering Foundation symposium proceedings","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.1007/2789_2007_032","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"","JCRName":"","Score":null,"Total":0}
Scale-up in microwave-accelerated organic synthesis.
Microwave-assisted organic chemistry has received strong exposure in the literature over the last decade, and nowadays more and more research chemists are successfully applying microwave technology to organic reactions on a small scale. However, the efficient application of this technology to cover the specific needs of larger-scale preparations, e.g., in a kilo lab, remains to be shown. We therefore initiated a study to investigate the scalability of microwave technology. Two different microwave systems designed for large-scale operation were evaluated in order to characterize strengths and weaknesses of each instrument with regard to scale-up. Special focus was directed on temperature/pressure limits, handling of suspensions, ability to rapidly heat and cool, robustness, and overall processing time. Based on the results of this study, a batch microwave reactor with a reaction volume of approximately 1.1 1 was purchased and installed in the kilo lab. Several reactions have been performed successfully on a 50- to 100-g scale in our laboratory, showing that a scale-up from a 15 ml scale to a 1-1 scale is feasible. In general, a significant reduction of reaction time was achievable, in some cases yields and selectivity were also improved. Nevertheless, a major weakness of the available systems is the limited vessel size, which is, in most cases, far below a suitable reaction volume required for work in a kilo lab.