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.

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.

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.
• Resolution of the enantiomers of 1-phenylethylamine.

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).

Workshops (weeks 1 - 11)

Each workshop will begin with a short lecture to introduce the topicscovered. Students will then work through problem sheets with the guidance of the demonstrators.

The following material will be covered

• Introduction to the physical basis of NMR. Quantum numbers, energy levels, magnetic equivalence, chemical shifts, scalar couplings. Revision of CHEM 111 material.
• The students will be asked to fill in the blanks for sequences of synthetic reaction schemes and explain the outcome and selectivity of reactions by use of the analytical data supplied to them. Interpretation of mass spectra, infrared spectra, elemental analyses and ¹H and ¹³C NMR spectra will be required to determine structures.
• Spin-spin coupling (J values) in ¹H NMR and their use in the de termination of stereochemistry and conformational analysis will be introduced.
• In the second part of the course, workshops will consist of a fifty-minute lecture introducing 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.
  
  

In this module students will be expected to complete a series of synthetic experiments. Each experiment will have a preliminary exercise (which includes a consideration of safety issues) which must be marked before the experiment is performed. On completion of the experiment, students must produce a writeup describing what was done and theri results. This must be marked before the next experiemnt in undertaken. The teaching Laboratory will be open for nine hours per week. Students will be expected to orgaise their own time to compete the necessary experiments.

The laboratory sessions are complemented by a series of workshops on spectroscopic tehcniques. Students are expected to work through a series of exercises with the support of teaching staff. The knowlegde gained in the workshops is tested by means of a class test at the end of the workshops.

"Organic Spectroscopy”, D.H.Williams and I. Fleming,Chapman and Hall, 1996.

“NMR Spectroscopy in Inorganic Chemistry”, J.A.Iggo, OUP, 1999.