Preparative enantioselective chromatography /

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Bibliographic Details
Imprint:	Ames, Iowa : Blackwell Pub., 2005.
Description:	xiv, 330 p. : ill. ; 26 cm.
Language:	English
Subject:	Liquid chromatography. Enantiomers -- Separation. Enantiomers -- Separation. Liquid chromatography.
Format:	Print Book
URL for this record:	http://pi.lib.uchicago.edu/1001/cat/bib/5778711

Hidden Bibliographic Details
Other authors / contributors:	Cox, Geoffrey J., 1952-
ISBN:	1405118709 (hardback : alk. paper)
Notes:	Includes bibliographical references and index.

Table of Contents:

Contributors
Preface
1. Chiral chromatography in support of pharmaceutical process research
1.1. Introduction
1.2. A brief introduction to chirality
1.3. Why chirality is important
1.4. Accessing enantiopurity: a brief overview of approaches
1.4.1. Enantiopure starting materials: the chiral pool
1.4.2. Removable enantioenriched auxiliaries
1.4.3. Enantioselective catalysis
1.4.4. Resolution technologies: introduction
1.4.5. Chromatographic productivity is the key metric for preparative chromatography
1.4.6. Stationary phases for preparative chiral chromatography
1.4.7. Advantages of preparative chiral chromatography over other approaches for accessing enantiopure materials
1.4.8. Simulated moving bed enantioseparation
1.5. Green enantioseparation
1.6. What is the appropriate role of preparative chromatography in organic synthesis?
1.7. Fording the river at the easiest point: some observations on the appropriate placement of a chromatographic resolution within a chiral synthesis
1.8. Origins of preparative chiral chromatography
1.9. Practical tips for preparative chromatographic enantioseparation
1.10. Conclusion
2. Introduction to preparative chromatography
2.1. Introduction
2.2. Adsorption isotherms
2.2.1. The simple case - the Langmuir isotherm
2.2.2. Other isotherms
2.2.3. Competitive isotherms
2.3. Kinetics
2.4. Metrics for preparative operations
2.4.1. Throughput
2.4.2. Production rate
2.4.3. Productivity
2.4.4. Specific productivity
2.4.5. Cost
2.5. The influence of chromatographic parameters on preparative chromatography
2.5.1. Effect of particle size on preparative performance
2.5.2. Effects of pressure
2.5.3. Effects of column efficiency
2.5.4. Effect of column length
2.5.5. The effects of selectivity
2.6. Economics of preparative separations
2.6.1. Point of insertion of the chromatographic resolution in the synthetic route
3. Chiral stationary phases for preparative enantioselective chromatography
3.1. Summary
3.2. Introduction
3.3. Historical development of CSPs for preparative chromatography
3.4. Preparative CSPs
3.4.1. Classification of CSPs
3.4.2. Polymeric phases
3.4.3. Brush-type CSPs
3.4.4. Chiral phases for ligand-exchange chromatography
3.4.5. Imprinted phases
3.5. Chemical and physical properties of CSPs
3.5.1. Loading capacity
3.5.2. Chemical and physical stability
3.5.3. Solubility of the chiral solute
3.6. New and future developments in the field of preparative CSPs
3.6.1. CSPs with improved loading capacity
3.6.2. CSPs with improved selectivity
3.6.3. Immobilised polysaccharide-based CSPs
3.7. Conclusion
4. Method development for preparative enantioselective chromatography
4.1. Introduction
4.2. Chiral stationary phases for enantioselective chromatography
4.3. Screening and optimisation strategy for preparative chiral chromatography
4.3.1. Choice of the stationary phase
4.3.2. Choice of the mobile phase
4.3.3. Screening and optimisation of specific phases
4.3.4. Additives in the mobile phase
4.4. Preparative separations, criteria and objectives
4.4.1. Loadability and productivity
4.4.2. Selectivity and productivity
4.4.3. Solubility and productivity
4.4.4. Viscosity and productivity
4.4.5. Chemical and enantiomeric stability
4.5. Scale-up issues
4.5.1. Laboratory-scale separations
4.5.2. Large-scale separations
4.6. Conclusion
5. Scaling-up of preparative chromatographic enantiomer separations
5.1. Introduction
5.2. Analytical screening models
5.2.1. Standard procedure
5.2.2. Fast analytical screening process
5.3. Scaling-up from milligram to kilogram quantities
5.3.1. Introduction
5.3.2. Separation of a xanthone derivative
5.3.3. Separation of 'dibenzocycloheptanol' derivative
5.3.4. Separation of a 'pyrido-pyrimidin-4-one' derivative
5.3.5. Separation of a piperazinyl-piperidine derivative
5.3.6. Summary - scale-up
5.4. Larger scale separations
5.4.1. Introduction
5.4.2. Separation of a 'pyrolidino-quinolinone' derivative
5.5. Scale-up problems in early development
5.5.1. Introduction
5.5.2. Separation of a 'tetracyclic' compound
5.5.3. Non-natural amino acids
5.5.4. Separation of an 'indole' derivative
5.5.5. Summary
5.6. General conclusions
6. Steady-state recycling and its use in chiral separations
6.1. Overview
6.2. Introduction
6.3. SSR - concept and operation
6.3.1. Concept
6.3.2. Operation
6.3.3. Role of the injection loop
6.4. Case studies
6.4.1. Case study 1
6.4.2. Case study 2
6.4.3. Case study 3: collection of three SSR fractions
6.5. Conclusions
7. Simulated moving bed and related techniques
7.1. Overview
7.2. The SMB concept
7.3. Modeling of SMB processes
7.4. Design of SMB processes
7.5. Simulation of SMB processes
7.5.1. Influence of the equilibrium adsorption isotherms
7.5.2. Influence of mass transfer resistance
7.6. SMB related techniques
7.6.1. Varicol processes
7.6.2. Pseudo-SMB processes
8. Preparative-scale supercritical fluid chromatography
8.1. Introduction
8.2. History of SFC at GlaxoSmithKline
8.3. Principles of SFC
8.4. Advantages of SFC
8.5. Drawbacks of preparative SFC
8.6. Use of SFC
8.7. Chiral separation using SFC
8.8. Achiral separation using SFC
8.9. Consideration of preparative SFC
8.10. Future direction and development
8.11. Conclusion
9. Equipment for preparative and large size enantioselective chromatography
9.1. Introduction
9.2. The heart of the chromatographic process: the column
9.2.1. Packing technique, bed formation and bed consolidation
9.2.2. The wall region
9.2.3. Heat dissipation
9.2.4. Column technology
9.2.5. Column design
9.3. Equipment considerations for batch chromatography
9.3.1. Recycling
9.3.2. Detection
9.4. Supercritical fluid chromatography
9.4.1. Principle
9.4.2. Technical aspects
9.4.3. Eluent
9.4.4. Pumping
9.4.5. Injection
9.4.6. Detection
9.4.7. Product recovery
9.4.8. Eluent recycling
9.4.9. High-pressure technology, safety aspects
9.5. Multicolumn continuous chromatographic processes
9.5.1. Simulated moving bed
9.5.2. VARICOL
10. Case study in production-scale multicolumn continuous chromatography
10.1. Introduction
10.2. Chromatographic process research
10.2.1. Introduction
10.2.2. Selection of racemate to separate
10.2.3. Choice of the chromatographic conditions
10.2.4. Choice of the separation technique
10.3. Process development
10.3.1. Optimisation of the chemical steps
10.4. Production facts
10.4.1. Introduction
10.4.2. Implementation in a cGMP production environment
10.4.3. Qualification
10.4.4. Validation
10.4.5. Production and maintenance data
10.5. Further areas of development
11. Contract manufacturing and outsourcing considerations
11.1. Introduction
11.2. The regulatory agencies and the chiral market
11.3. Contract manufacturing
11.3.1. Time constraints
11.3.2. Risk of capital investment
11.3.3. Expertise
11.3.4. Intellectual property
11.3.5. Location
11.3.6. Primary or secondary supplier
11.4. Selecting the outsourcing partner
11.4.1. Expectations
11.4.2. Audit
11.4.3. Decision grid
11.5. Communication
11.5.1. Contact matrix
11.5.2. Frequent updates
11.6. Project requirements
11.6.1. R&D - method development
11.6.2. Clinical trial quantities
11.6.3. Trial runs vs production runs
11.6.4. Commercial-scale quantities
11.6.5. Schedule
11.6.6. Quantity
11.6.7. Product quality
11.7. Transfer of information
11.7.1. Feed characterization
11.7.2. Separation conditions
11.7.3. The chiral stationary phase
11.7.4. Analytical methods
11.7.5. Impurity specifications
11.7.6. Final product
11.7.7. Other considerations
11.7.8. End of the project
11.8. Economics
11.8.1. Productivity
11.8.2. Production rate
11.8.3. Cost breakdown
11.8.4. Clinical trial quantities
11.8.5. Commercial-scale quantities
11.9. Conclusion
Appendix. Advanced concepts
Index

Preparative enantioselective chromatography /

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