Module Details

The information contained in this module specification was correct at the time of publication but may be subject to change, either during the session because of unforeseen circumstances, or following review of the module at the end of the session. Queries about the module should be directed to the member of staff with responsibility for the module.
Title PREPARATIVE CHEMISTRY: SYNTHESIS AND CHARACTERISATION
Code CHEM245
Coordinator Dr JW Gaynor
Chemistry
J.W.Gaynor@liverpool.ac.uk
Year CATS Level Semester CATS Value
Session 2016-17 Level 5 FHEQ First Semester 15

Pre-requisites before taking this module (or general academic requirements):

Completion of year 1 of either an MChem or a BSc (Hons) Chemistry programme.  

Aims

The module aims to present a unified approach to the synthesis and characterisation of organic, organometallic and inorganic compounds and will build on techniques introduced in the first year module CHEM111.


Learning Outcomes

By the end of the module students will

  • have completed a number of different types of experiment including the use of protecting groups in organic transformations, the use of metal ions as "templates" in organic synthesis and the synthesis of organometallic and classical complexes of the transition metals.
  • have experience of the use of spectroscopic techniques (UV, IR, NMR and mass spectrometry) in the characterisation of organic and inorganic compounds and will be able to use analytical and spectroscopic methods to characterise their synthesised compounds
  • be able to use word processing and chemical structure drawing programmes to produce written experimental reports.

Teaching and Learning Strategies

Laboratory Work -

Students can spend 2-3 sessions a week in the laboratory

Other -


Syllabus

1

Organic experiments (weeks 1-6)

Students are expected to complete satisfactorily three of the following experiments

  • A Hantzsch pyridine synthesis.
  • Synthesis of dimedone by carbonyl condensations.
  • A Grignard reaction using a protecting group.
  • Separation of fluorene/fluorenone using column chromatography

Inorganic experiments (weeks 7-12)

Students are expected to complete satisfactorily three preparations from

  • Preparation and analysis of iron(II) oxalate.
  • Preparation and analysis of acetylacetonato-complexes of transition-metals.
  • Preparation of a cobaltammine and the determination of its molecular formula.
  • Preparation and characterisation of a tetra-azamacrocycle complex of Ni(II).
  • Preparation of dichlorobis(ethylenediamine)cobalt(III) complex
  • Preparation of a metal-organic framework based around magnesium formate

Workshops (weeks 1 - 11)

There are a few themes discussed below. These will be taught using a variety of strategies including: mixed lecture and workshop sessions; working through problem sheets, either individually or in small groups, with the guidance of the demonstrators; and the use of online systems to aid learning.

The following material will be covered

  • Spectroscop y: Revision and expansion of various spectroscopic techniques including mass spectrometry, infrared spectra, ultraviolet spectroscopy, elemental analyses and NMR (1H and 13C). Spin-spin coupling (J values) in 1H NMR and their use in the determination of stereochemistry and conformational analysis will be introduced. Interpretation of mass spectra, infrared spectra, elemental analyses and 1H and 13C NMR spectra will be required to determine the structures of simple organic molecules.
  • Basic concepts in transition metal chemistry: In the second part of the course, workshops will consist of a fifty-minute lecture intro ducing basic concepts in transition metal chemistry and metal complex characterisation techniques, followed by guided worked examples. Material covered will include: introduction/revision of crystal field theory, spectroscopy and magnetism of transition metal ions and complexes; characterisation of complexes using analytical and spectroscopic techniques.
  • Lab based workshops: Students will delve into the underlying reasons behind certain practical techniques to deepen understanding in the laboratory.

Recommended Texts

Reading lists are managed at readinglists.liverpool.ac.uk. Click here to access the reading lists for this module.
Explanation of Reading List:

Teaching Schedule

  Lectures Seminars Tutorials Lab Practicals Fieldwork Placement Other TOTAL
Study Hours       90

  33

123
Timetable (if known)       Students can spend 2-3 sessions a week in the laboratory
 
     
Private Study 27
TOTAL HOURS 150

Assessment

EXAM Duration Timing
(Semester)
% of
final
mark
Resit/resubmission
opportunity
Penalty for late
submission
Notes
             
CONTINUOUS Duration Timing
(Semester)
% of
final
mark
Resit/resubmission
opportunity
Penalty for late
submission
Notes
Coursework    first  33  none  students are expected to complete the workshop material within the given time.  Assessment 1 
Coursework    First  67  No    Assessment 2 Notes (applying to all assessments) workshops This work is not marked anonymously laboratory work No deadlines for submission of reports, but students are responsible for completing enough experiments during semester. Work marked in students presence to allow for immediate feedback or students lab book marked. Anonymous marking impossible.