Chemicals, Reagents, and Solvents

Chemicals and reagents were obtained from commercial sources. Solvents were purified by standard techniques to give anhydrous solvents. Phosphorous trichloride, triethylamine, and thionyl chloride were distilled before use. Potassium fluoride, alumina, and sodium iodide were dried by oven before use. Thin layer chromatography (TLC) and column chromatography were performed on silica gel. 

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The correct disposal of chemicals, reagents and solvents is a matter of good laboratoiy practice and should comply with national and/or environmental and/or health safety regulations. 

Chemicals and Solvents. H2N-Met( SMe)2 and [ CJiodomethane were from Sigma Chemical Company. [Acetic-l- C]anhydride (9.20 mCi/mmol) was from NEN Research Products and [ HJacetic anhydride (6.94 Ci/mmol) was from Amersham Corp. All other chemicals, reagents and solvents were high purity preparations obtained from commercial sources. 

As with many separation processes, solvent extraction of metals was first developed as a tool of the analytical chemist. Chemical reagents and solvents are known for isolating virtually every metallic elemem of the Periodic Table. In the 1940s and 1950s some of this basic analytical chemistry was used to develop... 

Materials. The starting PPO was purchased from Aldrich Chemical Co. Two reprecipitations from chloroform into methanol served to purify the polymer. The bromine, chlorosulfonic acid, sulfonyl chlorides, acid chlorides as well as all other reagents and solvents were purchased from Aldrich Chemical Co. and were used without further purification. 

All other reagents and solvents were obtained from Kodak Laboratory Chemicals. All monomers were purified by distillation under an inert atmosphere. They were distilled from and collected over 3 A molecular sieves just prior to the polymerizations (11). TMSI was distilled under an inert atmosphere and stored over copper powder. 

The first step in the CSD process is solution preparation, which involves reagent selection (chemical precursors) and solvent choice.1,5-12,16 During solution preparation, other chemical modifiers may also be added to the solution to facilitate or limit chemical reactivity. Also during this stage of the process, identification of appropriate reaction conditions to promote other desired changes in precursor nature or solution characteristics is also considered. The goal for solution preparation is to develop a homogeneous solution of the necessary cation species that may later be applied to a substrate. 

All reagents and solvents that are used to prepare the sample for analysis should be ultrapure to prevent contamination of the sample with impurities. Plastic ware should be avoided since these materials may contain ultratrace elements that can be leached into the analyte solutions. Chemically cleaned glassware is recommended for all sample preparation procedures. Liquid samples can be analyzed directly or after dilution when the concentrations are too high. Remember, all analytical errors are multiplied by dilution factors therefore, using atomic spectroscopy to determine high concentrations of elements may be less accurate than classical gravimetric methods. 

Bromobenzaldehyde and triphenylphosphine were purchased from Aldrich Chemical Company, Inc. Benzeneboronic acid and palladium acetate were obtained from Lancaster Synthesis. Sodium carbonate was purchased from EM Science and deionized water was used to prepare the 2 M solution. Reagent grade 1-propanol is available from Mallinkrodt Inc. All reagents and solvents are used without purification or degassing. There was no need to dry the glassware rigorously. 

The obvious hazards in the syntheses reported in this volume are delineated, where appropriate, in the experimental procedure. It is impossible, however, to foresee every eventuality, such as a new biological effect of a common laboratory reagent. As a consequence, all chemicals used and all reactions described in this volume should be viewed as potentially hazardous. Care should be taken to avoid inhalation or other physical contact with all reagents and solvents used in this volume. In addition, particular attention should be paid to avoiding sparks, open flames, or other potential sources that could set fire to combustible vapors or gases. 

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