{"id":109,"date":"2015-05-06T11:36:48","date_gmt":"2015-05-06T15:36:48","guid":{"rendered":"http:\/\/caslabs.case.edu\/protasiewicz\/?page_id=109"},"modified":"2016-09-20T14:17:30","modified_gmt":"2016-09-20T18:17:30","slug":"technique","status":"publish","type":"page","link":"https:\/\/caslabs.case.edu\/protasiewicz\/chem-331\/technique\/","title":{"rendered":"Technique &amp; Information"},"content":{"rendered":"<hr \/>\n<p><span style=\"color: #000000\"><span style=\"color: #000080\"><strong>Comprehensive Organometallic Chemistry III<\/strong><\/span> has a great set of chapters on Experimental Methods and Techniques.\u00a0 In particular please see chapter 1.07 \u201cExperimental Methods and Techniques: Basic Techniques\u201d for details on vacuum and Schlenk techniques.\u00a0 This entire book is online and available via our library, and you can download each chapter as a pdf file. <\/span><\/p>\n<p><span style=\"color: #000000\"><span style=\"color: #000080\"><strong><a style=\"color: #000080\" title=\"http:\/\/www.sigmaaldrich.com\/chemistry\/chemical-synthesis\/learning-center\/technical-bulletins.html\" href=\"http:\/\/www.sigmaaldrich.com\/chemistry\/chemical-synthesis\/learning-center\/technical-bulletins.html\">Aldrich Technical Bulletins<\/a><\/strong><\/span> provide very useful and *free* guides for handling various types of chemicals, especially for air- and water-sensitive reagents.\u00a0 They also provide instructions for other types of operations.\u00a0 Bulletins <a style=\"color: #000000\" title=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al134.pdf\" href=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al134.pdf\">AL-134<\/a> and <a style=\"color: #000000\" title=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al164.pdf\" href=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al164.pdf\">Al-164<\/a> are of particular importance for CHEM 331 students for handling reagents.<\/span><\/p>\n<hr \/>\n<h3>Alison Frontier from the University of Rochester has a spectacular website <strong><a href=\"http:\/\/chem.chem.rochester.edu\/~nvd\/pages\/tips.php?page=about\">Not Vodoo X<\/a><\/strong> that is a gold mine of tips and techniques for practicing synthesis chemists. \u00a0A MUST SEE website!!<\/h3>\n<hr \/>\n<p><span style=\"color: #000000\"><span style=\"color: #000080\"><strong>How do you use that glassware and apparatus?<\/strong><\/span>\u00a0 Check out Rob Toreki\u2019s <a style=\"color: #000000\" title=\"http:\/\/www.ilpi.com\/inorganic\/glassware\/index.html\" href=\"http:\/\/www.ilpi.com\/inorganic\/glassware\/index.html\">Glassware Gallery<\/a>!\u00a0 Lots of good descriptions.<\/span><\/p>\n<hr \/>\n<p><span style=\"color: #000000\"><strong><span style=\"color: #000080\">How pure is your NMR spectrum?<\/span><\/strong>\u00a0 Please consult this great resource:\u00a0 Fulmer, G. R.; Miller, A. J. M.; Sherden, N. H.; Gottlieb, H. E.; Nudelman, A.; Stoltz, B. M.; Bercaw, J. E.; Goldberg, K. I., <a style=\"color: #000000\" title=\"http:\/\/pubs.acs.org\/doi\/abs\/10.1021\/om100106e\" href=\"http:\/\/pubs.acs.org\/doi\/abs\/10.1021\/om100106e\">NMR Chemical Shifts of Trace Impurities: Common Laboratory Solvents, Organics, and Gases in Deuterated Solvents Relevant to the Organometallic Chemist<\/a>. Organometallics 2010, 29 (9), 2176-2179.<\/span><\/p>\n<hr \/>\n<p><span style=\"color: #000080\"><strong>Titration of organometallic reagents-two different methods are used in this course:<\/strong><\/span><\/p>\n<ol>\n<li value=\"1\"><span style=\"color: #000000\">\u00a0\u201c<a style=\"color: #000000\" title=\"http:\/\/pubs.acs.org\/doi\/abs\/10.1021\/jo982433e\" href=\"http:\/\/pubs.acs.org\/doi\/abs\/10.1021\/jo982433e\">The use of salicylaldehyde phenylhydrazone as an indicator of organometallic reagents<\/a>\u201d by Brian E. Love and Edward G. Jones in the Journal of Organic Chemistry, 1999, 64, 3755-3756.<\/span><\/li>\n<li value=\"2\"><span style=\"color: #000000\">\u00a0\u201c<a style=\"color: #000000\" title=\"http:\/\/www.thieme-connect.com\/ejournals\/abstract\/synthesis\/doi\/10.1055\/s-2006-926345\" href=\"http:\/\/www.thieme-connect.com\/ejournals\/abstract\/synthesis\/doi\/10.1055\/s-2006-926345\">Convenient titration method for organometallic Zinc, Magnesium and Lanthanide reagents<\/a>\u201d by Arkady Krasovskiy and Paul Knochel in Synthesis, 2006, 890-891.<\/span><\/li>\n<\/ol>\n<p><span style=\"color: #000000\">In addition, there is a <a style=\"color: #000000\" title=\"http:\/\/www.chemistry.mcmaster.ca\/emslie\/Assets\/Titrating RLi.pdf\" href=\"http:\/\/www.chemistry.mcmaster.ca\/emslie\/Assets\/Titrating%20RLi.pdf\">great handout<\/a> Prof. David Emslie at the McMaster University has prepared discussing the titration of these types of reagents that should definitely be consulted.\u00a0 Thanks David!.<\/span><\/p>\n<hr \/>\n<h4><span style=\"color: #000080\"><strong>Got Dry Solvents?\u00a0 <\/strong><\/span><\/h4>\n<p><span style=\"color: #000000\">A nice series of papers are listed below in which the authors took the time and effort to actually measure the efficacy of various drying methods for different solvent types.<\/span><\/p>\n<p><span style=\"color: #000000\">Desiccant efficiency in solvent drying. A reappraisal by application of a novel method for solvent water assay<\/span><br \/>\n<span style=\"color: #000000\">David R. Burfield, Kim-Her Lee, Roger H. Smithers<\/span><br \/>\n<span style=\"color: #000000\"><em>Journal of Organic Chemistry<\/em> <strong>1977,<\/strong> <em>42<\/em> (18), 3060-3065\u00a0 <\/span><\/p>\n<p><span style=\"color: #000000\">\u00a0\u00a0\u00a0\u00a0\u00a0\u00a0\u00a0 Good for solvents such as <a style=\"color: #000000\" title=\"http:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jo00438a024\" href=\"http:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jo00438a024\">Acetontrile, Benzene, and Dioxane<\/a><\/span><\/p>\n<p><span style=\"color: #000000\">Desiccant efficiency in solvent drying. 3. Dipolar aprotic solvents<\/span><br \/>\n<span style=\"color: #000000\">David R. Burfield, Roger H. Smithers<\/span><br \/>\n<span style=\"color: #000000\"><em>Journal of Organic Chemistry<\/em> <strong>1978,<\/strong> <em>43<\/em> (20), 3966-3968<\/span><\/p>\n<p><span style=\"color: #000000\">\u00a0\u00a0\u00a0\u00a0\u00a0\u00a0\u00a0 Good for dipolar solvents such as <a style=\"color: #000000\" title=\"http:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jo00414a038\" href=\"http:\/\/pubs.acs.org\/doi\/pdf\/10.1021\/jo00414a038\">HMPT and DMP<\/a>: <\/span><\/p>\n<p class=\"Body\"><span style=\"color: #000000\"><span class=\"style_17\">Desiccant efficiency in solvent and reagent drying. 7. Alcohols<\/span><span class=\"style_18\"><br \/>\n<\/span><span class=\"style_19\">David R. Burfield, Roger H. Smithers<br \/>\n<\/span><em><span class=\"style_20\">Journal of Organic Chemistry<\/span><\/em> <strong><span class=\"style_18\">1983,<\/span><\/strong> <em><span class=\"style_20\">48<\/span><\/em><span class=\"style_19\"> (14), 2420-2422<br \/>\n<\/span><\/span><\/p>\n<p class=\"Body\"><span class=\"style_19\" style=\"color: #000000\">\u00a0\u00a0\u00a0\u00a0\u00a0\u00a0<\/span><\/p>\n","protected":false},"excerpt":{"rendered":"<p><strong>Comprehensive Organometallic Chemistry III<\/strong> has a great set of chapters on Experimental Methods and Techniques.\u00a0 In particular please see chapter 1.07 \u201cExperimental Methods and Techniques: Basic Techniques\u201d for details on vacuum and Schlenk techniques.\u00a0 This entire book is online and available via our library, and you can download each chapter as a pdf file. <\/p>\n<p><strong><a style=\"color: #000080\" title=\"http:\/\/www.sigmaaldrich.com\/chemistry\/chemical-synthesis\/learning-center\/technical-bulletins.html\" href=\"http:\/\/www.sigmaaldrich.com\/chemistry\/chemical-synthesis\/learning-center\/technical-bulletins.html\">Aldrich Technical Bulletins<\/a><\/strong> provide very useful and *free* guides for handling various types of chemicals, especially for air- and water-sensitive reagents.\u00a0 They also provide instructions for other types of operations.\u00a0 Bulletins <a style=\"color: #000000\" title=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al134.pdf\" href=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al134.pdf\">AL-134<\/a> and <a style=\"color: #000000\" title=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al164.pdf\" href=\"http:\/\/www.sigmaaldrich.com\/etc\/medialib\/docs\/Aldrich\/Bulletin\/al_techbull_al164.pdf\">Al-164<\/a> are of particular importance for CHEM 331 students for handling reagents.<\/p>\n<p><a href=\"https:\/\/caslabs.case.edu\/protasiewicz\/chem-331\/technique\/\" class=\"more-link\">Continue reading&#8230; <span class=\"screen-reader-text\">Technique &amp; Information<\/span><\/a><\/p>\n","protected":false},"author":122,"featured_media":0,"parent":83,"menu_order":0,"comment_status":"open","ping_status":"open","template":"","meta":{"spay_email":""},"_links":{"self":[{"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/pages\/109"}],"collection":[{"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/pages"}],"about":[{"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/types\/page"}],"author":[{"embeddable":true,"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/users\/122"}],"replies":[{"embeddable":true,"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/comments?post=109"}],"version-history":[{"count":10,"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/pages\/109\/revisions"}],"predecessor-version":[{"id":437,"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/pages\/109\/revisions\/437"}],"up":[{"embeddable":true,"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/pages\/83"}],"wp:attachment":[{"href":"https:\/\/caslabs.case.edu\/protasiewicz\/wp-json\/wp\/v2\/media?parent=109"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}