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Experiment 7 Procedure.docx

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CHEM 235
Dana Zendrowski

Experiment 7 Procedure 1) Put 15 mL amyl alcohol & 20 mL acetic acid into 100 mL RB flask 2) Add 3 mL sulfuric acid, little at a time while swirling 3) Add boiling chip and set up system for reflux (20 minutes) a. See pg A-63 – observe where clamp is placed in setup 4) During reflux: a. Pre-weigh 3 large test tubes w/ cork (in beaker; tare beaker first) b. Cool test tubes in large beaker ice bath c. Get/clean large separatory funnel d. Collect all wash solvents for extraction 5) Remove heat source and let mixture cool for few minutes then ice bath 6) Once cooled, transfer to separatory funnel a. Note: i. Make sure stopcock is closed ii. Place a beaker underneath iii. Before extracting, remember to remove stopper iv. At end of extractions, collect top layer into separate flask and cork! 7) Wash organic layer with 2 X 25 mL H O 2 8) Wash organic layer with 2 x 15 mL 5% NaHCO (rele3se pressure more often) 9) Check aqueous layer to see if its basic in last wash a. If acidic: wash once more with NaHCO 3 10) Wash organic layer with 15 mL saturated NaCl 11) Pour ester into dry 50 mL E. flask and dry w/ MgSo f4r 10 minutes a. Add until free grains seen, tighten cork and swirl 12) Calibrate thermometer a. Prepare ice bath in 400 mL beaker, place thermometer and wait b. Place small drop of glycerol at tip and insert into
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