Practical Process Research & Development
Regular price
59.250 KD
inc. VAT
Couldn't load pickup availability
Table of contents
- Contentsvii
- Foreword by K. Barry Sharplessxv
- Foreword by Jerome L. Moniotxix
- Prefacexxi
- About the Authorxxiii
- Chapter 1. Approaches to Process Development1
- I. Introduction1
- II. The Importance of Simple Scale-up Operations5
- III. The Importance of Teamwork8
- IV. Determining Operations That Can and Cannot Readily Be Used On Scale8
- V. Safety Considerations19
- VI. Taking Advantage of Serendipity and Good Observations20
- VII. Define the Time Available for Process Optimization21
- References24
- Chapter 2. Route Selection27
- I. Introduction27
- II. Characteristics of Expedient Routes28
- III. Characteristics of Cost-Effective Routes30
- IV. Using Cost Estimates to Assess the Ultimate Route46
- V. Summary50
- References50
- Chapter 3. Reagent Selection53
- I. Introduction53
- II. The Ideal Reagent for Scale-up53
- III. Families of Reagents Useful for Scale-up61
- References78
- Chapter 4. Solvent Selection81
- I. Introduction81
- II. Selecting Solvents Based on Physical Characteristics83
- III. Selected Solvent Impurities89
- IV. Applications of Solvents91
- V. Alternatives to Classical Solvents102
- References108
- Chapter 5. Running the Reaction113
- I. Introduction113
- II. Determining Reaction Safety113
- III. Assessing Safe Operating Conditions for the Laboratory115
- IV. Selecting the Reaction Scale116
- V. Choose Equivalents of Reagents, Starting Materials, and Solvents117
- VI. Employ Inert Conditions if Needed121
- VII. Charge Starting Materials and Solvents122
- VIII. Select Reaction Temperature122
- IX. Select the Duration and Temperature of an Addition124
- X. Select the Sequence of Additions128
- XI. Select Reaction Pressure129
- XII. Adjust Stirring131
- XIII. Monitor the Reaction Conditions132
- References133
- Chapter 6. Effects of Water135
- I. Introduction135
- II. Detecting and Quantitating Water136
- III. Removing Water from Routine Organic Processing137
- References143
- Chapter 7. In-Process Controls145
- I. Introduction145
- II. Choosing the Appropriate IPC148
- III. Generating Reproducible IPCs154
- References163
- Chapter 8. Optimizing the Reaction by Minimizing Impurities165
- I. Introduction165
- II. Steps to Optimizing Reactions168
- III. Minimizing Impurity Formation by Identifying Impurities First179
- IV. Statistical Design of Experiments180
- V. Robotics and Automated Process Optimization182
- References183
- Chapter 9. Optimizing Catalytic Reactions185
- I. Introduction185
- II. Catalyst Selection/Ligand Selection187
- III. Optimizing Catalyst Concentration188
- IV. Generating Active Catalysts191
- V. Importance of Extended Additions192
- VI. Influence of Co-catalysts and Impurities193
- VII. Catalyst Decomposition196
- VIII. Nonlinear Catalyst Effects196
- IX. The Difficulty of Optimizing a Catalytic Reaction197
- References199
- Chapter 10. Work-up203
- I. Introduction203
- II. Aspects of Work-up204
- References220
- Chapter 11. Tools for Purifying the Product: Column Chromatography, Crystallization, and Reslurrying223
- I. Introduction223
- II. Purification by Column Chromatography224
- III. Crystallization226
- IV. Purification by Reslurrying243
- References245
- Chapter 12. Final Product Form and Impurity Considerations249
- I. Introduction249
- II. The Importance of Solid State Characteristics251
- III. Preparing and Selecting the Polymorph256
- IV. Purity and Impurity Considerations: Freezing the Final Process259
- References265
- Chapter 13. Vessels and Mixing269
- I. Introduction269
- II. Batch vs. Continuous Processing272
- III. Use of Continuous Flow Reactors to Scale up Processes281
- References288
- Chapter 14. Preparing for and Implementing the Scale-up Run291
- I. Introduction291
- II. Anticipating Scale-up Problems292
- III. Scale-up Considerations294
- IV. Implementing the Scale-up Run302
- References311
- Chapter 15. Troubleshooting313
- I. Introduction313
- II. Physical and Chemical Causes of Processing Problems314
- III. Steps for Troubleshooting a Process319
- IV. Debottlenecking a Problem327
- References328
- Chapter 16. Chiral Syntheses329
- I. Introduction329
- II. Some Examples of Molecules Prepared by Asymmetric Synthesis330
- III. Compounds Prepared by Asymmetric Synthesis337
- IV. Perspective on Asymmetric Synthesis341
- References342
- General Index345
- Reaction Type Index351
- Reagent Index353
This book provides a comprehensive, step-by-step approach to organic process research and development in the pharmaceutical, fine
chemical, and agricultural chemical industries. Process R&D describes the steps taken, following synthesis and evaluation, to bring key
compounds to market in a cost-effective manner. More people are being hired for work in this area as increasing numbers of drug candidates are
identified through combinatorial chemistry and high-throughput screening. The book is directed to industrial (primarily organic) chemists, and
academicians (particularly those involved in a growing number of start-up companies) and students who need insight into industrial process R&D. Current books do not describe hands-on, step-by-step, approaches to solving process development problems, including route, reagent,
and solvent selection; optimising catalytic reactions; chiral syntheses; and "green chemistry." "Practical Process Research and Development" will be a valuable resource for researchers, managers, and graduate students.
* Provides insights into generating rugged, practical, cost-effective processes for the chemical preparation of "small molecules"
* Breaks down process optimization into route, reagent and solvent selection, development of reaction conditions, workup, crystallizations and more
* Includes over 100 tips for rapid process development
* Presents guidelines for implementing and troubleshooting processes
chemical, and agricultural chemical industries. Process R&D describes the steps taken, following synthesis and evaluation, to bring key
compounds to market in a cost-effective manner. More people are being hired for work in this area as increasing numbers of drug candidates are
identified through combinatorial chemistry and high-throughput screening. The book is directed to industrial (primarily organic) chemists, and
academicians (particularly those involved in a growing number of start-up companies) and students who need insight into industrial process R&D. Current books do not describe hands-on, step-by-step, approaches to solving process development problems, including route, reagent,
and solvent selection; optimising catalytic reactions; chiral syntheses; and "green chemistry." "Practical Process Research and Development" will be a valuable resource for researchers, managers, and graduate students.
* Provides insights into generating rugged, practical, cost-effective processes for the chemical preparation of "small molecules"
* Breaks down process optimization into route, reagent and solvent selection, development of reaction conditions, workup, crystallizations and more
* Includes over 100 tips for rapid process development
* Presents guidelines for implementing and troubleshooting processes