{"title":"利用原甲酸三乙酯作为原位脱水剂提高二氯双（三苯基膦）镍（II）及相关化合物的产率：对一个经典本科生无机合成的合理改进","authors":"Adrian R. Hilts, and , Jason Cooke*, ","doi":"10.1021/acs.jchemed.3c00637","DOIUrl":null,"url":null,"abstract":"<p >The addition of a small excess of triethyl orthoformate to an alcoholic mixture of NiCl<sub>2</sub>·6H<sub>2</sub>O and triphenylphosphine (PPh<sub>3</sub>) results in an increase in the typical isolated yield of [NiCl<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>] from below 50% to over 85%. The impact of water when present in the reaction medium in this system is discussed, and results from the application of the same synthetic approach to the syntheses of [NiBr<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>], [NiCl<sub>2</sub>(dppe)], and [NiBr<sub>2</sub>(dppe)] are presented. A simple synthesis of NiCl<sub>2</sub>·2H<sub>2</sub>O by the dehydration of NiCl<sub>2</sub>·6H<sub>2</sub>O at 80 °C can be performed as an optional step to decrease the quantity of triethyl orthoformate required for the preparation of [NiCl<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>] and/or [NiCl<sub>2</sub>(dppe)]. The experiments are flexible and accommodate a variety of laboratory schedules and student skill levels. Each synthesis can be readily completed within a 3 h laboratory period.</p>","PeriodicalId":43,"journal":{"name":"Journal of Chemical Education","volume":"100 10","pages":"4119–4121"},"PeriodicalIF":2.5000,"publicationDate":"2023-09-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Improved Yields of Dichlorobis(triphenylphosphine)nickel(II) and Related Compounds by Employing Triethyl Orthoformate as an In Situ Dehydrating Agent: Rational Improvement of a Classic Undergraduate Inorganic Synthesis\",\"authors\":\"Adrian R. Hilts, and , Jason Cooke*, \",\"doi\":\"10.1021/acs.jchemed.3c00637\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >The addition of a small excess of triethyl orthoformate to an alcoholic mixture of NiCl<sub>2</sub>·6H<sub>2</sub>O and triphenylphosphine (PPh<sub>3</sub>) results in an increase in the typical isolated yield of [NiCl<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>] from below 50% to over 85%. The impact of water when present in the reaction medium in this system is discussed, and results from the application of the same synthetic approach to the syntheses of [NiBr<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>], [NiCl<sub>2</sub>(dppe)], and [NiBr<sub>2</sub>(dppe)] are presented. A simple synthesis of NiCl<sub>2</sub>·2H<sub>2</sub>O by the dehydration of NiCl<sub>2</sub>·6H<sub>2</sub>O at 80 °C can be performed as an optional step to decrease the quantity of triethyl orthoformate required for the preparation of [NiCl<sub>2</sub>(PPh<sub>3</sub>)<sub>2</sub>] and/or [NiCl<sub>2</sub>(dppe)]. The experiments are flexible and accommodate a variety of laboratory schedules and student skill levels. Each synthesis can be readily completed within a 3 h laboratory period.</p>\",\"PeriodicalId\":43,\"journal\":{\"name\":\"Journal of Chemical Education\",\"volume\":\"100 10\",\"pages\":\"4119–4121\"},\"PeriodicalIF\":2.5000,\"publicationDate\":\"2023-09-07\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chemical Education\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.acs.org/doi/10.1021/acs.jchemed.3c00637\",\"RegionNum\":3,\"RegionCategory\":\"教育学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chemical Education","FirstCategoryId":"92","ListUrlMain":"https://pubs.acs.org/doi/10.1021/acs.jchemed.3c00637","RegionNum":3,"RegionCategory":"教育学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
Improved Yields of Dichlorobis(triphenylphosphine)nickel(II) and Related Compounds by Employing Triethyl Orthoformate as an In Situ Dehydrating Agent: Rational Improvement of a Classic Undergraduate Inorganic Synthesis
The addition of a small excess of triethyl orthoformate to an alcoholic mixture of NiCl2·6H2O and triphenylphosphine (PPh3) results in an increase in the typical isolated yield of [NiCl2(PPh3)2] from below 50% to over 85%. The impact of water when present in the reaction medium in this system is discussed, and results from the application of the same synthetic approach to the syntheses of [NiBr2(PPh3)2], [NiCl2(dppe)], and [NiBr2(dppe)] are presented. A simple synthesis of NiCl2·2H2O by the dehydration of NiCl2·6H2O at 80 °C can be performed as an optional step to decrease the quantity of triethyl orthoformate required for the preparation of [NiCl2(PPh3)2] and/or [NiCl2(dppe)]. The experiments are flexible and accommodate a variety of laboratory schedules and student skill levels. Each synthesis can be readily completed within a 3 h laboratory period.
期刊介绍：
The Journal of Chemical Education is the official journal of the Division of Chemical Education of the American Chemical Society, co-published with the American Chemical Society Publications Division. Launched in 1924, the Journal of Chemical Education is the world’s premier chemical education journal. The Journal publishes peer-reviewed articles and related information as a resource to those in the field of chemical education and to those institutions that serve them. JCE typically addresses chemical content, activities, laboratory experiments, instructional methods, and pedagogies. The Journal serves as a means of communication among people across the world who are interested in the teaching and learning of chemistry. This includes instructors of chemistry from middle school through graduate school, professional staff who support these teaching activities, as well as some scientists in commerce, industry, and government.
求助内容：
应助结果提醒方式：
京公网安备 11010802042870号
