2311 lec 12 - Nitration of Methyl Benzoate Objective...

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Nitration of Methyl Benzoate
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Objective Perform small scale (mini) Synthesis Learn the technique of Recrystallization Use TLC to analyze reaction and crystallization Analyze product by mpt Analyze product by IR Analyze product by NMR Confirm substitution pattern using J values of ortho, meta, para hydrogens
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Procedure TestTube A - 1 mL sulfuric acid cooled (CAUTION!) Add ~ 0.5 g methyl benzoate MIX WELL (important for reaction) TestTube B – 0.35 mL nitric + 0.35 mL sulfuric acid Add dropwise to A keeping temp below 15 o C Allow to warm to rt + 15 minutes Pour onto ice Product separates as a solid Vacuum filter crude Æ mass, save some for TLC Recrystallize – MeOH/water solvent pair
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Recrystallization Mohrig – Technique 9 Most Common Method of purifying an organic solid Slow, selective process (versus precipitation which is fast and often not selective allowing impurities)
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Steps of Crystallization (p. 106) 1. Dissolve Solid 1 or 2 solvent mixture where solute is soluble HOT but insoluble COLD 2. Remove insoluble impurities – (hot filtration) 3. Crystallize – allow to cool.
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2311 lec 12 - Nitration of Methyl Benzoate Objective...

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