Flow synthesis

A method of electrochemical continuous flow synthesis of N-nitrosamines by nitrosylation of amines is provided, the method comprising the steps of (i) preparing input flow reagent A comprising an amine of Formula (I) as defined herein in a first solvent,; (ii) preparing input flow reagent B a nitrit...

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Bibliographische Detailangaben
Hauptverfasser: Rebecca Elizabeth Stevens, Rojan Ali, Thomas Writh, Matthew Paul Didsbury
Format: Patent
Sprache:eng
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Zusammenfassung:A method of electrochemical continuous flow synthesis of N-nitrosamines by nitrosylation of amines is provided, the method comprising the steps of (i) preparing input flow reagent A comprising an amine of Formula (I) as defined herein in a first solvent,; (ii) preparing input flow reagent B a nitrite salt in an aqueous solution; (iii) causing the input flow reagent A and B to enter a continuous electrochemical flow reactor provided with electrodes for electrolysis, at a flow rate, to provide a reaction solution comprising a N-nitrosamine of Formula II as defined herein. The formation of N-nitroso-N-methybenzylamine from N-methylbenzylamine with sodium nitrite is exemplified. Piperazine, pyrrolidine, azepane, morpholine and thiomorpholine can all be used as the amine in the electrochemical flow nitrosylation reaction. A method of electrochemical continuous flow nitrosylation of amines for the synthesis of N-nitrosamines is provided. A method of synthesising N-nitramines by electrochemical continuous flow comprising the steps of (xv) selecting an N-nitrosamine in a first solvent; (xvi) causing the N-nitrosamine to be subject to continuous flow electrochemical oxidation to form a N-nitramine is provided. The N-nitramine formed may be an energetic material such as RDX, HMX or CL20.