{"title":"用CaBr2沉淀法轻松去除反应混合物中的氧化三苯基膦","authors":"Antonio Rodríguez Hergueta*, ","doi":"10.1021/acs.oprd.2c00104","DOIUrl":null,"url":null,"abstract":"<p >A reliable and scalable purification procedure for the easy removal of triphenylphosphine oxide by complexation with CaBr<sub>2</sub> in ethereal solvents or toluene was developed. The resulting insoluble precipitated complex was easily eliminated from crude reaction mixtures in high yields by filtration without the need of purification by column chromatography. The compatibility of this procedure with different organic solvents, salts, filtration aids, packing materials, and several molecules containing most common organic functional groups was examined to explore the scope and limitations of this method. Additionally, precipitation of TPPO by complexation with other halide salts was also explored.</p>","PeriodicalId":55,"journal":{"name":"Organic Process Research & Development","volume":null,"pages":null},"PeriodicalIF":3.1000,"publicationDate":"2022-06-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"1","resultStr":"{\"title\":\"Easy Removal of Triphenylphosphine Oxide from Reaction Mixtures by Precipitation with CaBr2\",\"authors\":\"Antonio Rodríguez Hergueta*, \",\"doi\":\"10.1021/acs.oprd.2c00104\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >A reliable and scalable purification procedure for the easy removal of triphenylphosphine oxide by complexation with CaBr<sub>2</sub> in ethereal solvents or toluene was developed. The resulting insoluble precipitated complex was easily eliminated from crude reaction mixtures in high yields by filtration without the need of purification by column chromatography. The compatibility of this procedure with different organic solvents, salts, filtration aids, packing materials, and several molecules containing most common organic functional groups was examined to explore the scope and limitations of this method. Additionally, precipitation of TPPO by complexation with other halide salts was also explored.</p>\",\"PeriodicalId\":55,\"journal\":{\"name\":\"Organic Process Research & Development\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":3.1000,\"publicationDate\":\"2022-06-09\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"1\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Organic Process Research & Development\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acs.oprd.2c00104\",\"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.2c00104","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, APPLIED","Score":null,"Total":0}
Easy Removal of Triphenylphosphine Oxide from Reaction Mixtures by Precipitation with CaBr2
A reliable and scalable purification procedure for the easy removal of triphenylphosphine oxide by complexation with CaBr2 in ethereal solvents or toluene was developed. The resulting insoluble precipitated complex was easily eliminated from crude reaction mixtures in high yields by filtration without the need of purification by column chromatography. The compatibility of this procedure with different organic solvents, salts, filtration aids, packing materials, and several molecules containing most common organic functional groups was examined to explore the scope and limitations of this method. Additionally, precipitation of TPPO by complexation with other halide salts was also explored.
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.
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