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15 Pre Lab - lab work
lab work
Course
Organic Chemistry Lab II (CHEM201401)
46 Documents
Students shared 46 documents in this course
University
Boston College
Academic year: 2017/2018
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College of the Holy Cross
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- 0 g of benzyl in 50 mL Erlenmeyer flask. Then add 5 mL of 95% ethanol. Swirl flask and cool under running water to produce a fine suspension. 0 g sodium borohydride and swirl. Let it sit for 10 minutes (solution should be clear and yellow color should fade in 2- 3 minutes). Add 5 mL of water and heat to boiling point on steam bath. If solution isn’t clear, filter by gravity (hot) through fluted filter paper. Add 10 mL of water to solution and set it aside to crystalize. Use vacuum filtration to collect. Obtain melting point and mass next week. Oxidation.
- 1 g of isoborneol in 3 mL of glacial acetic acid in 50 mL Erlenmeyer flask. Swirl to dissolve solid. 8 mL of bleach to flask all at once and swirl. It will precipitate immediately. Continue to swirl the flask occasionally for 15 minutes.
- Moisten starch-iodine paper with a drop or two of 6 M of HCl. Place one drop of the supernatant on paper. If paper turns dark blue, excess Hypochlorous acid is present and reaction is complete. If it doesn’t turn blue, add another 0-1 mL of bleach and swirl and let it sit for 5 minutes. Test solution with paper again.
- Once completed, add 30 mL of water to flask and transfer contents to sep funnel. 30 mL of diethyl ether to funnel and use little to rinse flask. Add 2 mL of saturated sodium bisulfite solution and swirl. If you want to test, get paper and see if it turns blue (shouldn’t). shake contents for 25 seconds.
- Drain lower layer from sep. Wash ether layer two times with 10 mL of saturated sodium bisulfite. The funnel needs to be vented frequently. Lower layer discard. After second portion is added, shake until gas is no longer evolved. And drain. Organic layer goes into Erlenmeyer flask. Dry the organic layer (ether) with sodium sulfate. Decant the dried solution through plug of cotton into 40 mL vial. Evaporate most of solvent using centrifan. When volume is 4-5 mL (1 cm), remove vial.
- Pour solution from vial into tared side arm 125 mL filter flask. Small amont of ether to rinse the vial. Add to filter flask. Place #5 rubber stopper to mouth and attach vacuum. Slowly open valve. Turn off as soon all the liquid has evaporated (or the product will sublime). Weigh.
- Purify by sublimation set up apparatus. Position 13x100 mm test tube in adaptor so it doesn’t touch side of bottom of flask. Place filter flask in thermowell and turn on heat. Place ice in the test tube and wrap the flask with foil. Do not hook up flask to vacuum. Cover the opening of side arm with foil. When bottom is empty of solid material, turn off heat. Scrape the camphor off the test tube into a tared weighing paper and get mass. Measure melting point.
- Place spatula tip to small test tube and add minimum amount of CH2Cl and stir to dissolve. (10-15) and if doesn’t dissolve, then let it sit at bottom.
- IR: salt plate. Three drops. Move plate as solvent evaps, and that the solid is deposited on surface.
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15 Pre Lab - lab work
Course: Organic Chemistry Lab II (CHEM201401)
46 Documents
Students shared 46 documents in this course
University: Boston College
Was this document helpful?
1. 0.5 g of benzyl in 50 mL Erlenmeyer flask. Then add 5 mL of 95% ethanol. Swirl flask and
cool under running water to produce a fine suspension. 0.1 g sodium borohydride and
swirl. Let it sit for 10 minutes (solution should be clear and yellow color should fade in 2-
3 minutes). Add 5 mL of water and heat to boiling point on steam bath. If solution isn’t
clear, filter by gravity (hot) through fluted filter paper. Add 10 mL of water to solution
and set it aside to crystalize. Use vacuum filtration to collect. Obtain melting point and
mass next week.
Oxidation.
2. 1.0 g of isoborneol in 3 mL of glacial acetic acid in 50 mL Erlenmeyer flask. Swirl to
dissolve solid. 8 mL of bleach to flask all at once and swirl. It will precipitate immediately.
Continue to swirl the flask occasionally for 15 minutes.
3. Moisten starch-iodine paper with a drop or two of 6 M of HCl. Place one drop of the
supernatant on paper. If paper turns dark blue, excess Hypochlorous acid is present and
reaction is complete. If it doesn’t turn blue, add another 0.5-1 mL of bleach and swirl
and let it sit for 5 minutes. Test solution with paper again.
4. Once completed, add 30 mL of water to flask and transfer contents to sep funnel. 30 mL
of diethyl ether to funnel and use little to rinse flask. Add 2 mL of saturated sodium
bisulfite solution and swirl. If you want to test, get paper and see if it turns blue
(shouldn’t). shake contents for 25 seconds.
5. Drain lower layer from sep. Wash ether layer two times with 10 mL of saturated sodium
bisulfite. The funnel needs to be vented frequently. Lower layer discard. After second
portion is added, shake until gas is no longer evolved. And drain. Organic layer goes into
Erlenmeyer flask. Dry the organic layer (ether) with sodium sulfate. Decant the dried
solution through plug of cotton into 40 mL vial. Evaporate most of solvent using
centrifan. When volume is 4-5 mL (1 cm), remove vial.
6. Pour solution from vial into tared side arm 125 mL filter flask. Small amont of ether to
rinse the vial. Add to filter flask. Place #5 rubber stopper to mouth and attach vacuum.
Slowly open valve. Turn off as soon all the liquid has evaporated (or the product will
sublime). Weigh.
7. Purify by sublimation set up apparatus. Position 13x100 mm test tube in adaptor so it
doesn’t touch side of bottom of flask. Place filter flask in thermowell and turn on heat.
Place ice in the test tube and wrap the flask with foil. Do not hook up flask to vacuum.
Cover the opening of side arm with foil. When bottom is empty of solid material, turn off
heat. Scrape the camphor off the test tube into a tared weighing paper and get mass.
Measure melting point.
8. Place spatula tip to small test tube and add minimum amount of CH2Cl and stir to
dissolve. (10-15) and if doesn’t dissolve, then let it sit at bottom.
9. IR: salt plate. Three drops. Move plate as solvent evaps, and that the solid is deposited
on surface.
