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Grignard Rxn - Amy Linkous CHEM 2556 CRN 91653 Grignard...

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Amy Linkous 9/9/09 CHEM 2556: CRN: 91653 Grignard Reaction: Synthesizing of Dye Objective: To use a Grignard reaction to synthesize triphenylmethane dye. General Reaction: Procedure: A drying tube was prepared prior to the reaction using a cotton plug and anhydrous calcium chloride. An apparatus for reflux was set up and the drying tube was positioned on top of the condenser using a thermometer adaptor. About 2.5 grams of magnesium ribbon was obtained and polished with the provided abrasive (sandpaper) until shiny, then cut into small pieces into a previously oven-dried round-bottom flask. 10 mL of dry THF was added to cover the magnesium, along with one iodine crystal. The flask was stoppered and clamped over a hot plate on low heat to warm.
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2.0 grams of 4-bromo- N,N -dimethylaniline was placed in a separate round-bottom and dissolved in the minimum amount of dry THF needed, which was approximately 3.0 mL. A small amount of this new solution was transferred into the warmed magnesium solution via pipette, then the warm solution was re-stoppered and gently swirled. Gaseous carbon dioxide
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