Practical courses in Medicinal Chemistry II
Timetable
●every even Thursday 13.00 – 20.30
●
September 19th
– December 12th
, 2013
●7 lessons
●punctuality is necessary !
●no absences will be tolerated
Organisation
● cycle of 6 exercises: 5 synthetic + 1 physico-
chemical
● work in pairs
● 2 pairs perform the same task at the particular
lesson (but different versions of the same task
are possible)
● every pair begins with the exercise chosen by
the lecturer at the first lesson and continues
with exercises in consecutive order
● if the exercise No. 6 is reached the pair continues
with the exercise No. 1
Requirements to get the credit
● complete attendance
● products in appropriate amounts and purity
● complete reports with appropriate data and
attachments
● spectra charts and their interpretations
● chromatograms
– ratio of peak areas of acetylsalicylic and salicylic acids
– retention times and factors
● yields in g and %
● melting points
● absorbance or specific absorption values
● at least 60 % success in tests
Reminder of elementary safety rules
● wear laboratory coat
● do not wear jewels, rings, bracelets etc.
● smoking is strictly forbidden in all the university
buildings
● eat and drink in a laboratory is forbidden
● long or artificial nails are not recommended
● every oil bath which is heated must contain a
thermometer
● every apparatus containing a stand must be
placed on its stand
Reminder of elementary safety rules - continued
● power cords and tubing must not touch hotplates or
heated baths
● water input into a condenser is from bottom, output from
top
● allow the cooling water flow only with smaller stream
● check ends of tubing which are connected either to the
condenser or to the water tap if they are not damaged
● work with chloroacetyl chloride and ethereal hydrogen
chloride must be performed in a fume hood
● volumes of liquids are measured with volumetric cylinders
or with pipettes equipped with pipette fillers (controllers)
● all other safety rules which you have listened in other
chemical disciplines remain valid
Where you will find your material and equipment and
where you will work?
● Equipment for you is placed in lockers and drawers with
blue numbers and letters (e.g. 5a – 5d), keys can be
found at the hanger outside the left fume hood
● You will work at the desk in which your lockers and
drawers are placed
● If your equipment is placed in lockers and drawers under
a window (21 and 23), you will work at the nearest
working desk (not at the table under the window)
● Chemicals are placed in the left side fume hood or at a
side of working desks
● Sodium is given cut into smaller parts by the laboratory
assistant into a dry flask filled with the appropriate volume
of propan-2-ol; you have to ask him
List of particular exercises
Exercise
No.
Table or
locker No. /
Place
Name of the exercise Outcomes needed in
addition to reports
1 1 + 3 Calcium dobesilate UV spectrum, specific
absorbance at aprox.
301 nm
2 7 + 9 Lidocaine interpreted IR spectrum,
TLC, melting point
3 5 + 23 Acetylsalicylic acid TLC and HPLC
chromatogrammes,
retention parameters,
approx. purity, melting
point
4 13 + 15 Phenytoin TLC
5 11 + 21 Parabens TLC, interpreted 1HNMR
spectrum, melting
point
6 Laboratory
No. 345
opposite
pKa
of phenytoin pKa
, UV spectra with
table of absorbances,
answers of additional
tasks
At the start, during and at the end of a practical lesson ...
● Before you begin your work, check the content of the
locker and the drawers of your working desk using the list
placed inside the door of the locker; tell the laboratory
assistant or the teacher about the potential deficiency in
equipment immediately
● If you break or damage any piece of laboratory glass,
report it immediately to laboratory assistant together with
your name
● After you have finished your work, contact the laboratory
assistant and let him (her) check your working desk
● Reports of your tasks are continuously checked at the end
of every lesson in a preliminary form and definitely before
recording the credit
● Finally they must contain all the requirements listed in
above table (identity date, interpreted spectra etc.)