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A.

Kepustakaan
B. Prosedur
Sumber: Funnis BS, et al, 1978, Vogels Textbook of Practical Organic Chemistry, 4 th
edition, The English Language Book Society and Longman, London, 813-832
Conversion to acetylsalicylic acid (aspirin). Place 10 gram (0,725 mol) of dry salicylic
acid and 15 gram (114 ml. 0,147 mol) of acetic anhydride in a small conical flask, add 5
drops of concentrated sulphuric acid and rotate the flask in order to secure thorough
mixing. Warm on a water bath to about 50-60C, stirring with a thermometer, for about 15
minutes. Allow the mixture to cool and stir occasionally. Add 150 ml of water, stir well
and filter at the pump. Dissolve the warm water: if a solid separates at this point, warm the
mixture until solution is complete and then allow the clear solution to cool slowly.
Beautiful needle-like crystals will separate. The yield is 11 gram (85). The air-dried crude
product may also be recrystallised from ether-light petroleum (b.p. 40-60C).
Acetylsalicylic acid decomposes when heated and does not posses a true clearly
defined m.p. Decomposition points varying from 128 to 135C have been recorded: a
value of 129-133C is obtained on an electric hot plate(Fig.1,162). Some decomposition
may occur if the compound is recrystallised from a solvent of high boiling point or if the
boiling period during recrystallisation is unduly prolonged.
C. Dasar Teori
D. Tujuan
1. Mampu memahami dan menjelaskan reaksi asetilasi.
2. Mampu melakukan pemurnian aspirin dengan cara rekristalisasi menggunakan 2
pelarut campuran dengan terampil.
E. Bahan
Asam salisilat
: 5 gram
Anhidrida asetat : 7 ml
H2SO4 pekat
: 3 tetes
FeCl3
: 2-3 tetes
Aquadem
: 75 ml
Etanol panas
: 15 ml
Aquadem panas : 37,5 ml
F. Alat
a. Erlenmeyer 250 ml
l. Kertas perkamen
b. Termometer
m. Kertas saring
c. Kaca arloji
n. Kapas
d. Corong Buchner
o. Sumbat gabus
e. Labu hisap
p. Pipet tetes
f. Pompa hisap
q. Corong biasa
g. Pengaduk
r. Hot plate
h. Gelas ukur
s. Timbangan gram
i. Oven
t. Magnetic bar
j. Anak timbangan + pinset
u. Penangas air + Bunsen
k. Beaker glass

G. Mekanisme Reaksi

H. Cara Kerja
I. Skema Kerja
J.

Gambar Pemasangan Alat

3
2
1

Erlenmeyer 250 ml

H2SO4 pekat 3 tetes


Anh.
asetat
7
ml
Asam salisilat 5 gram

FeCl3

digoyang-goyang ad tercampur sempurna

Padatan

diaduk sampai dingin dan


terbentuk padatan

tidak berwarna ungu

dipanaskan di penangas dengan


suhu 50oC - 60oC selama 5-10
menit

Jika
berwarna
ungu
maka
dipanaskan lagi

segera

Air aquadest 75 ml

Diaduk dan dikocok kuat


penghisap
padatan yang sudah disaring
dimasukkan
dalam
erlenmeyer yang baru
1
2
kapas

45
3
21

ditunggu sampai dingin dan


terbentuk kristal

45
3
21

67
8
11
9

45
3
2
1

67
8
11
9

45
3
2
1

67
8
9
1
0

etanol panas 15 ml

67
8
9
1
0

dikocok dengan magnetic


stirer di atas hot plate
air panas 37,5 ml

kaca arloji

corong buchner
disaring dengan corong Buchner

keringkan
dibalik cepat, bila perlu
dengan meniup pelan
tanpa
kontak
dengan
mulut

dimasukkan oven ad kering

K.
L.
M.
N.

Hasil Percobaan
Ketetapan Alam
Pembahasan dan Diskusi
xx

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