For the set up of the extraction apparatus in the microwave see
article "Microwave: Extraction".
In each of the inner glass vials of the apparatus, 3-5 g
nutmeg powder,
a magnetic stir bar and 40 mL
ethanol
are placed. A further 40 mL ethanol are filled in between the inner vials and
the outer wall.
Setting parameters:
The program Easywave® is opened on the PC and the following parameters are set:
t1 (time to reach the set temperature):
5 min
t2 (time at set temperature):
10 min
T0:
room temperature
T1 (set temperature):
120 °C
P1 (power in step 1):
700 W
P2 (power in step 2):
500 W
Work up
The recovered ethanol extracted is stored overnight in the refrigerator. The
precipitated trimyristin is filtered using a funnel or a small frit and then
dried. If the crystals are not colourless, the crude product is recrystallized
from ethanol.
Crude product yield: 0.6-0.9 g; melting point 54-55 °C;
Colourless, very fine crystals
The filtrate is concentrated on the rotary evaporator, leaving a light brown
oil. The following fatty acids can be identified in this oil, after
transesterification with methanolic potassium hydroxide: Capronic acid,
tridecanoic acid, myristin acid, pentadecanoic acid, palmitin acid,
cis-10-heptadecenoic acid and oleic acid.
Duration of the experiment
Without recrystallization 1 hour
Where can I stop the experiment?
Almost at any time, as long as the solvent is taken out of the reaction vials whilst still hot
Recycling
The evaporated ethanol is collected and redistilled