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Safe and High Yielding Flow Nitration Methodology
Uniqsis has published details of a mild nitration method using its FlowSyn flow chemistry system that enables short reaction times and high conversion to be achieved whilst minimising the amount of corrosive (and potentially explosive) hot nitrating mixture present in the reactor at any one time.
Nitration is an important synthetic procedure that is often difficult to control. Under continuous flow-through conditions, however, exotherms are typically well controlled and nitration can be safely performed on a large scale. Using Uniqsis’s proprietary glass static mixer/reactor chip technology - nitration can be safely performed under accelerated conditions at elevated temperature and pressure without the associated problems typically encountered in batch reactors of controlling latency periods or controlling thermal run away.
Application Note 22 describes how the Uniqsis FlowSyn™ flow chemistry system fitted with a glass static mixer/reactor chip can be used to undertake rapid, high yield nitration of methyl 3-methoxy, 4-ethoxybenzoate using nitric acid and acetic acid by the method described above. The product was conveniently isolated in high yield and purity by precipitation from water.
The Uniqsis FlowSyn™ is a compact integrated continuous flow reactor system designed for easy, safe and efficient operation. The FlowSyn™ range includes models for performing single or multiple homogeneous or heterogeneous reactions, either manually or automatically. The range of chemistries that can be explored with Uniqsis’ integrated and modular flow chemistry systems grows ever wider and is exemplified by the growing number of applications published both in the academic press and in Uniqsis’ own application notes. Typical examples of flow chemistry applications include hydrogenation, nitration, bromination, metalation, molecular rearrangements and synthesis of compounds suchas dihyropyridine, indole, pyrazole, quinolinone and benzimidazole.
Uniqsis specialises in the design of meso-scale continuous flow chemistry systems for a wide range of applications in chemical and pharmaceutical research. The company’s aim is to make flow chemistry easily accessible to both novices and experienced users.