Extraction (Part 2) Experiment: Separation of Neutral and basic Substances NH2 Handle aromatic amines with care. Most are toxic and some are carcinogenic. Avoid breathing the dust and vapor from the solid and keep the compounds off the skin, best done by wearing gloves. Naphthalene mp 80°C 4-Chloroaniline mp 68–71°C, pK, 10.0 1) Dissolve 2g of mixture in 20 mL of ethyl ether, and transfer the mixture to a 125 mL separatory funnel. 2) Add 10 mL of H,O and 10 mL of a 3M HCl solution into the funnel. 3) Stopper the funnel, shakes the mixture thoroughly with frequent venting of the funnel. 4) Allow the layers to separate completely, then draw off the lower layer into a 50 mL flask (flask 1) 5) Repeat the process with another 10 mL of HCl. Draw off the lower layer into flask 1. Correct positions for holding a separatory funnel when shaking. FIG. 3

Organic Chemistry
8th Edition
ISBN:9781305580350
Author:William H. Brown, Brent L. Iverson, Eric Anslyn, Christopher S. Foote
Publisher:William H. Brown, Brent L. Iverson, Eric Anslyn, Christopher S. Foote
Chapter16: Aldehydes And Ketones
Section: Chapter Questions
Problem 16.39P
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Create a detailed flow sheet for the following experiment.
6) Add 15 mL of a saturated NaCl solution to separatory funnel, shake,
allow the layer to separate. Draw off the lower layer. Carefully pour the
ether layer into a 50 ml of flask (flask 2). Add about 4g of anhydrous
CaCl, and let it aside.
7) Dropwise addition of NaOH into flask 1, until no more solid coming
out, cool the flask with ice bath.
8) Decant the ether layer from flask 2 into a new beaker taking care to
leave all of solid behind. Then evaporated.
9) Collect the solid from flask 1 by suction filtration
10) Weight all the two compounds and test m.p.
FIG. 4 Separatory funnel with
Teflon stopcock.
Transcribed Image Text:6) Add 15 mL of a saturated NaCl solution to separatory funnel, shake, allow the layer to separate. Draw off the lower layer. Carefully pour the ether layer into a 50 ml of flask (flask 2). Add about 4g of anhydrous CaCl, and let it aside. 7) Dropwise addition of NaOH into flask 1, until no more solid coming out, cool the flask with ice bath. 8) Decant the ether layer from flask 2 into a new beaker taking care to leave all of solid behind. Then evaporated. 9) Collect the solid from flask 1 by suction filtration 10) Weight all the two compounds and test m.p. FIG. 4 Separatory funnel with Teflon stopcock.
Extraction (Part 2)
Experiment: Separation of Neutral and basic Substances
NH2
Handle aromatic amines
with care. Most are toxic
and some are carcinogenic.
Avoid breathing the dust
and vapor from the solid
and keep the compounds off
the skin, best done by
wearing gloves.
Naphthalene
mp 80°C
4-Chloroaniline
mp 68-71°C, рк, 10.0
1) Dissolve 2g of mixture in 20 mL of ethyl ether, and transfer the
mixture to a 125 mL separatory funnel.
2) Add 10 mL of H,O and 10 mL of a 3M HCl solution into the funnel.
3) Stopper the funnel, shakes the mixture thoroughly with frequent
venting of the funnel.
4) Allow the layers to separate completely, then draw off the lower layer
into a 50 mL flask (flask 1)
5) Repeat the process with another 10 mL of HCl. Draw off the lower
layer into flask 1.
Correct positions for
holding a separatory funnel
when shaking.
FIG. 3
Transcribed Image Text:Extraction (Part 2) Experiment: Separation of Neutral and basic Substances NH2 Handle aromatic amines with care. Most are toxic and some are carcinogenic. Avoid breathing the dust and vapor from the solid and keep the compounds off the skin, best done by wearing gloves. Naphthalene mp 80°C 4-Chloroaniline mp 68-71°C, рк, 10.0 1) Dissolve 2g of mixture in 20 mL of ethyl ether, and transfer the mixture to a 125 mL separatory funnel. 2) Add 10 mL of H,O and 10 mL of a 3M HCl solution into the funnel. 3) Stopper the funnel, shakes the mixture thoroughly with frequent venting of the funnel. 4) Allow the layers to separate completely, then draw off the lower layer into a 50 mL flask (flask 1) 5) Repeat the process with another 10 mL of HCl. Draw off the lower layer into flask 1. Correct positions for holding a separatory funnel when shaking. FIG. 3
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