Comprehensive Organometallic Chemistry III has a great set of chapters on Experimental Methods and Techniques. In particular please see chapter 1.07 “Experimental Methods and Techniques: Basic Techniques” for details on vacuum and Schlenk techniques. This entire book is online and available via our library, and you can download each chapter as a pdf file.
Aldrich Technical Bulletins provide very useful and *free* guides for handling various types of chemicals, especially for air- and water-sensitive reagents. They also provide instructions for other types of operations. Bulletins AL-134 and Al-164 are of particular importance for CHEM 331 students for handling reagents.
Alison Frontier from the University of Rochester has a spectacular website Not Vodoo X that is a gold mine of tips and techniques for practicing synthesis chemists. A MUST SEE website!!
How do you use that glassware and apparatus? Check out Rob Toreki’s Glassware Gallery! Lots of good descriptions.
How pure is your NMR spectrum? Please consult this great resource: Fulmer, G. R.; Miller, A. J. M.; Sherden, N. H.; Gottlieb, H. E.; Nudelman, A.; Stoltz, B. M.; Bercaw, J. E.; Goldberg, K. I., NMR Chemical Shifts of Trace Impurities: Common Laboratory Solvents, Organics, and Gases in Deuterated Solvents Relevant to the Organometallic Chemist. Organometallics 2010, 29 (9), 2176-2179.
Titration of organometallic reagents-two different methods are used in this course:
- “The use of salicylaldehyde phenylhydrazone as an indicator of organometallic reagents” by Brian E. Love and Edward G. Jones in the Journal of Organic Chemistry, 1999, 64, 3755-3756.
- “Convenient titration method for organometallic Zinc, Magnesium and Lanthanide reagents” by Arkady Krasovskiy and Paul Knochel in Synthesis, 2006, 890-891.
In addition, there is a great handout Prof. David Emslie at the McMaster University has prepared discussing the titration of these types of reagents that should definitely be consulted. Thanks David!.
Got Dry Solvents?
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.
Desiccant efficiency in solvent drying. A reappraisal by application of a novel method for solvent water assay
David R. Burfield, Kim-Her Lee, Roger H. Smithers
Journal of Organic Chemistry 1977, 42 (18), 3060-3065
Good for solvents such as Acetontrile, Benzene, and Dioxane
Desiccant efficiency in solvent drying. 3. Dipolar aprotic solvents
David R. Burfield, Roger H. Smithers
Journal of Organic Chemistry 1978, 43 (20), 3966-3968
Good for dipolar solvents such as HMPT and DMP:
Desiccant efficiency in solvent and reagent drying. 7. Alcohols
David R. Burfield, Roger H. Smithers
Journal of Organic Chemistry 1983, 48 (14), 2420-2422