|
Lecturer(s)
|
-
Dostál Libor, prof. Ing. Ph.D.
|
|
Course content
|
The aim of the course is to acquaint students with new demanding synthetic methods, especially with regard to work in an inert atmosphere using the so-called Schlenk technique in combination with the technique of septum and cannula. The aim is to master the work with vacuum-inert lines, which will allow them to work with highly sensitive compounds to air humidity and oxygen. Another object is to obtain the ability to dry various organic solvents and deprive them of oxygen residues, which is necessary to master the above technique. Preparations of other air-sensitive preparations, their isolation and characterization, according to current needs (control in the form of protocols). Within these laboratories, students will get acquainted with individual working groups in the workplace and their scientific focus, which will allow them to clarify the choice of their direction in solving the thesis in the future (ie the choice of a specific working group and supervisor). Checking theoretical knowledge in the form of written work focused on the above laboratory techniques and drying of solvents. Week 1: Introduction to health and safety + fire regulations. Week 2: Introduction to the principles of drying solvents using flow columns and standard techniques and their storage. Week 3-5: Organic syntheses of starting ligands used in the workplace, in particular substituted aromatics and cyclopentadienes eg 1,3- (Me2NCH2) 2C6H4, 1-Br-2,6- (RNCH) 2C6H3, C5H5 (SiMe3) and next. Week 6-9: Basic syntheses of organometallic and complex derivatives of non-transition elements, eg Ph4Sn, Ph3SnCl, [(Me3Si) 2N] 2Ge and [(Me3Si) 2N] 2Sn, 2,6- (RNCH) 2C6H3BiCl2 and 2,6- ( RNCH) 2C6H3SbCl2 and others. Week 10-12: Basic syntheses of organometallic derivatives of transition elements, eg ferrocene, its acetylation and other derivatives, synthesis of cyclopentadienyl complexes of transition metals derived from Ti, Mn, V. Week 13: Written work + submission of all protocols for the semester.
|
|
Learning activities and teaching methods
|
|
Laboratory work
|
|
Learning outcomes
|
Within the laboratories, the student will get acquainted with advanced techniques of chemical synthesis, with emphasis on the preparation and characterization of compounds in a very pure state and compounds sensitive to air humidity and air gases. The technique of Schlenk flasks, cannulae, septum and vacuum technique will be theoretically and practically discussed, as well as the drying of solvents and work at low temperatures. During the course, the student will learn and improve in the process leading from the literature, through the synthesis of starting compounds, the strategy of preparation of target products to their identification and determination of purity. The aim of the course is to educate students capable of independent laboratory work in an inert atmosphere.
The student will obtain the knowledge how to synthesize organometallic and inorganic compounds sensitive to moisture and oxygen, to characterize them and to perform the future research and use.
|
|
Prerequisites
|
unspecified
|
|
Assessment methods and criteria
|
Written examination
|
|
Recommended literature
|
-
Eisch J.J. Organometallic Syntheses, Vol.2, Nontransition-Metal Compounds, Part IA.. Academic Press, 1981.
-
Hanzlík J. Celoskleněná stavebnicová aparatura pro práci v inertní atmosféře. Chem. Listy 66(1972)628-642..
-
Herzog S., Dehnert J. Eine rationele anaerobe Arbeitsmethode. Z.Chem.4(1964)1-11.. 1964.
-
Keil B. a kol. Laboratorní technika organické chemie.. Praha (nakl. ČSAV), 1963.
-
Nádvorník M., Handlíř K. Návody pro laboratorní cvičení z předmětu Chemie organokovových sloučenin.. Pardubice, 2000.
|