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In a 50ml round-bottomed flask place 9 ml of 1 - butanol, 24ml of glacial acetic acid (ethanoic acid), and 3 ml of conc, Sulphuric acid. Add a boiling chip, and set up the flask for refluxing over a Bunsen burner (see refluxing techniques) and reflux for one hour. NOTE - use a gentle flame, and always place an asbestos or ceramic mat under the burner in order to protect the bench top. At the end of the reflux period, cool the flask by swirling gently in a beaker of cold water for 2-3 minutes. Transfer the reaction mixture to a separating funnel, and add 20ml of ice-cold water. Check that there are no burners in use on your entire bench, the measure out and add 20ml ether to the separating funnel, shake carefully, using some of the ether to rinse out the boiling flask. Stopper the funnel, and allow the layers to separate. Drain off the lower, aqueous layer. Wash the ether layer with a further 10ml water, then 10ml of 20% aqueous sodium carbonate solution (CAUTION - pressure building due to vigorous evolution of CO2 gas), discarding the lower, aqueous layer each time. Decant the ether layer into a clean, dry boiling tube and dry using anhydrous sodium sulphate. When the ether is dry, carefully decant into a dry 100ml conical flask, add a boiling chip, and WORKING IN THE FUME HOODS, carefully evaporate off the ether on a steam bath. Transfer the residual liquid to a clean, dry 25 ml round- bottomed flask. Set up the flask for distillation (all apparatus must be dry), and carefully purify the product by distillation (CAUTION - flammable product), collecting the fraction boiling above 1300C into a clean, dry, pre-weighed sample bottle. DO NOT distil to dryness. Record the mass of a pure ester obtained, and it's boiling range. yeild. .... Calculate the percentage

In a 50ml round-bottomed flask place 9 ml of 1 - butanol, 24ml of glacial acetic acid (ethanoic acid), and 3 ml of conc, Sulphuric acid. Add a boiling chip, and set up the flask for refluxing over a Bunsen burner (see refluxing techniques) and reflux for one hour. NOTE - use a gentle flame, and always place an asbestos or ceramic mat under the burner in order to protect the bench top. At the end of the reflux period, cool the flask by swirling gently in a beaker of cold water for 2-3 minutes. Transfer the reaction mixture to a separating funnel, and add 20ml of ice-cold water. Check that there are no burners in use on your entire bench, the measure out and add 20ml ether to the separating funnel, shake carefully, using some of the ether to rinse out the boiling flask. Stopper the funnel, and allow the layers to separate. Drain off the lower, aqueous layer. Wash the ether layer with a further 10ml water, then 10ml of 20% aqueous sodium carbonate solution (CAUTION - pressure building due to vigorous evolution of CO2 gas), discarding the lower, aqueous layer each time. Decant the ether layer into a clean, dry boiling tube and dry using anhydrous sodium sulphate. When the ether is dry, carefully decant into a dry 100ml conical flask, add a boiling chip, and WORKING IN THE FUME HOODS, carefully evaporate off the ether on a steam bath. Transfer the residual liquid to a clean, dry 25 ml round- bottomed flask. Set up the flask for distillation (all apparatus must be dry), and carefully purify the product by distillation (CAUTION - flammable product), collecting the fraction boiling above 1300C into a clean, dry, pre-weighed sample bottle. DO NOT distil to dryness. Record the mass of a pure ester obtained, and it's boiling range. yeild. .... Calculate the percentage

Chemistry
Chemistry
10th Edition
ISBN:9781305957404
Author:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Publisher:Steven S. Zumdahl, Susan A. Zumdahl, Donald J. DeCoste
Chapter1: Chemical Foundations
Section: Chapter Questions
Problem 1RQ: Define and explain the differences between the following terms. a. law and theory b. theory and...
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In a 50ml round-bottomed flask place 9 ml of 1 - butanol, 24ml of glacial acetic acid (ethanoic acid), and 3 ml of conc, Sulphuric acid. Add a boiling chip, and set up the flask for refluxing over a Bunsen burner (see refluxing techniques) and reflux for one hour. NOTE - use a gentle flame, and always place an asbestos or ceramic mat under the burner in order to protect the bench top. At the end of the reflux period, cool the flask by swirling gently in a beaker of cold water for 2-3 minutes. Transfer the reaction mixture to a separating funnel, and add 20ml of ice-cold water. Check that there are no burners in use on your entire bench, the measure out and add 20ml ether to the separating funnel, shake carefully, using some of the ether to rinse out the boiling flask. Stopper the funnel, and allow the layers to separate. Drain off the lower, aqueous layer. Wash the ether layer with a further 10ml water, then 10ml of 20% aqueous sodium carbonate solution (CAUTION - pressure building due to vigorous evolution of CO2 gas), discarding the lower, aqueous layer each time. Decant the ether layer into a clean, dry boiling tube and dry using anhydrous sodium sulphate. When the ether is dry, carefully decant into a dry 100ml conical flask, add a boiling chip, and WORKING IN THE FUME HOODS, carefully evaporate off the ether on a steam bath. Transfer the residual liquid to a clean, dry 25 ml round- bottomed flask. Set up the flask for distillation (all apparatus must be dry), and carefully purify the product by distillation (CAUTION - flammable product), collecting the fraction boiling above 1300C into a clean, dry, pre-weighed sample bottle. DO NOT distil to dryness. Record the mass of a pure ester obtained, and it's boiling range. yeild. .... Calculate the percentage
Transcribed Image Text:In a 50ml round-bottomed flask place 9 ml of 1 - butanol, 24ml of glacial acetic acid (ethanoic acid), and 3 ml of conc, Sulphuric acid. Add a boiling chip, and set up the flask for refluxing over a Bunsen burner (see refluxing techniques) and reflux for one hour. NOTE - use a gentle flame, and always place an asbestos or ceramic mat under the burner in order to protect the bench top. At the end of the reflux period, cool the flask by swirling gently in a beaker of cold water for 2-3 minutes. Transfer the reaction mixture to a separating funnel, and add 20ml of ice-cold water. Check that there are no burners in use on your entire bench, the measure out and add 20ml ether to the separating funnel, shake carefully, using some of the ether to rinse out the boiling flask. Stopper the funnel, and allow the layers to separate. Drain off the lower, aqueous layer. Wash the ether layer with a further 10ml water, then 10ml of 20% aqueous sodium carbonate solution (CAUTION - pressure building due to vigorous evolution of CO2 gas), discarding the lower, aqueous layer each time. Decant the ether layer into a clean, dry boiling tube and dry using anhydrous sodium sulphate. When the ether is dry, carefully decant into a dry 100ml conical flask, add a boiling chip, and WORKING IN THE FUME HOODS, carefully evaporate off the ether on a steam bath. Transfer the residual liquid to a clean, dry 25 ml round- bottomed flask. Set up the flask for distillation (all apparatus must be dry), and carefully purify the product by distillation (CAUTION - flammable product), collecting the fraction boiling above 1300C into a clean, dry, pre-weighed sample bottle. DO NOT distil to dryness. Record the mass of a pure ester obtained, and it's boiling range. yeild. .... Calculate the percentage
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