Abstract
This chapter focuses on the preparation, purification, and storage of solvents and reagents used in chemical syntheses. The tetrahydrofuran (THF) is mostly used in many syntheses. This solvent sometimes contains peroxides and small amounts of water especially after a long period of careless storage. For most of the procedures the THF, dried over potassium hydroxide (KOH), is used after rapid filtration. THF is best stored in a brown flask under inert gas, preferably argon. Purification is carried out by distillation from commercial potassium-tert-butoxide (t-BuOK) in a high vacuum followed by redistillation at 5–20 Torr (bp ∼110°C/15 Torr). Dry benzene, dichloromethane, chloroform, carbon tetrachloride, and alkyl halides are obtained by liquid distillation under normal pressure until a clear condense flows through the condenser. Chloroform and carbon tetrachloride are used as solvents for NMR spectroscopy. They are prepared by shaking with a very small amount of aqueous potassium carbonate, dried over the anhydrous salt and finally distilled. These are stored in brown bottles under inert gas. The chapter also discusses the procedures for preparation of various reagents.
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