Collect bottom layer and discard in aqueous waste container
Drain ether layer into Erlenmeyer flask, add anhydrous sodium sulfate to dry organic layer, let stand for few minutes
Filter drying agent into tared 125 mL vacuum flask, rince drying agent with fresh diethyl ether, add to vacuum flask
Vaporize ether with vacuum pump evaporator until sold remains
Measure weight of crude napthalene.
Determine products' melting points, and compare with literature value to comment on purity.
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Dissolve 3g solid mixture of equal quantities of benzoic acid, 4-chloroaniline, and napthalene in 30 ml of diethyl ether in erlenmeyer flask; transfer fluid to 125 mL separatory funnel
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Add 30 mL of 5% HCl, cap funnel, shake, unscrewing slightly to vent
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Allow two phases to separate into distinct layers, remove lower layer drawing it to 125 mL Erlenmeyer flask (flask 1) through separatory funnel
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Rinse product with cold ice water, dry them, and proceed with experiment
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Cool flask in ice, let stand for 15 minutes, collect precipitate formed by vacuum filtration
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Add 20 mL of NaCl sol'n to organic layer in separatory funnel to remove residual water present
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Add 6M HCl to acidify flask 2, cool flask 2 in ice bath. Check if acidic with pH paper. Collect precipitate via vacuum filtration, wash with ice water similar to efore. Dry product, and proceed.
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Draw off aqueous layer into erlenmeyer flask (flask 2)
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Add 50 mL of 5% NaOH to the ether solution; cap, shake, and vent as before
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Steadily dd 3M NaOH (check to be sure sol'n is basic)
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Collect bottom layer and discard in aqueous waste container
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Drain ether layer into Erlenmeyer flask, add anhydrous sodium sulfate to dry organic layer, let stand for few minutes
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Filter drying agent into tared 125 mL vacuum flask, rince drying agent with fresh diethyl ether, add to vacuum flask
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Vaporize ether with vacuum pump evaporator until solid remains
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Measure weight of crude napthalene.
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Determine products' melting points, and compare with literature value to comment on purity.
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Procedures
