31 of 47 31

2. Mount the reflux condenser on the top of the flask and warm the mixture in a water bath

till solution.
3. Pour the solution into ca. 75 ml of hot water. If the product crystallized at this stage, you
should dissolve it one more time in water bath.
4. Leave the solution for slow cooling.
5. Filter the crude product using vacuum filtration technique.
6. Place the product into evaporator and protect it with paper assigned to you.
7. Place the evaporator with dry product into a desiccator and leave until the next class.

Identity and purity determination:

Analytical test for phenols
1. In four clean and dry test tubes, dissolve salicylic acid, crude aspirin, recrystallized aspirin
and a sample of commercial drug in 2 ml of distilled water.
2. Add 2 - 3 drops of 2.5% water solution of iron(III) chloride. Watch and note down the color
of the solutions at the time of mixing reagents.

Purity determination of aspirin

1. Prepare a sample for NMR measurements: Place 3 - 5 mg of recrystallized aspirin in NMR
tube and add 0.6 ml of CDCl 3 • The group should additionally prepare two samples of crude
product and commercially available drug.
2. With the assistance of your teaching assistant (TA) go to NMR laboratory and collect NMR
spectra of your samples.
3. Compare NMR spectra you collected with those of your colleagues.

Reagents

Reagent 1 Reagent 2 catalyst Solvent

S~e, ~c H1SOl'1
name
Q,cid.,
<lt-Ul,

,o~-h1 qg;.~ tG, •O'f-

l?,g. i?l
,.
Molar weight (g/mol] 1

density (g/ml[
, • i+)J-'<, I· 21:) O"f-8%
mass/volume
IOo. IJ+M~
,fwdlfl/G
\NII- ~2,0mJ-
Melting point/ boiling f5g l>C, -=t'3·1 •e, 10-31 oc, II.LJ-.l 0 C.

I
 32

point

Safety information

Equipment (fill in the boxes)

I~
/
- I ~~c,ut

- 1<,:>~\I'

Observations and conclusions

Salt~cit-e, ctc.t'c.<. + o.c.w:c.,

- c.,,J,,u,tL pr1-ctp<..UA.lt -f6~.
I - prr.uptJ:uJ.e, chssoLJ-U) C,n a..cl.cLi/Jg

~){- 01) ~d CU: •G0° C..

' - [<; ,'\M.,") c oG v-L~~ Ctt-pw.JJ.i K-ct. sdW:Q_
v? ~ -
- ~,,, t~~) o.uJ;t.r.. cau.'d +
- a..c.&Dc ~ctvido. fua..ct aaiJJc. a~ cl
 33

Identity and purity determination

est for phenols
Test tube
4

compound
c.tw.Lt, fC.D"j6iu.W=~ ~f"t(.'o.l_
a.sflN' c:l-6pvv>
Color after
addition of FeCl 3

Description of product
uut,,w.:tvi ~I--\
~"'
Molar weight [g/mol)

mass[g)

yield[%]

Theoretical melting point

Analysis of NMR data

1,1.J.J:kw- Macjl\tb.C... ( t ~ ~ (,01'-1~) ""--l.pS:

(~ -S~ cJ-b a,,,-v,.pc./l-vlcA-, YI ct_

~co.l S ~ J pv, I ~rn---.u C'lq_

~tn,

e-<. lwl.cl& ct NM fZ fvr \+I

t~c I '"1'.J ) '"lf 11'\d ... ,o
I .
V\ AM fJMR. ""'"'-'-At. ·v·-<S=ct

-to c:b.twv-t. ~ ·co.t .rt.u.fj{ db . 1N. f'

OM~ ~ w l t k'{}t v., a.fW.cb.al ('(..cvY'Vn c:Jf) ~ C l . k

O; fv CAcl O'\.c:.l W'S~ • "NS NlpS Cl

~~ci,o..~a;l.w,
c>-v-,,:CcJl siu,lrt (4 Oil a.lr,...-,uc..