Following an organic synthesis reaction using Anton Paar’s Cora 5001 Raman spectrometer

The synthesis of acetylsalicylic acid is monitored using Anton Paar’s Cora 5001 Fiber benchtop Raman spectrometer together with a high temperature fiber probe.

Introduction

Chemical synthesis as an essential tool for creating new molecules and materials is used in various fields of application. Among the key tasks in synthesis are elucidating the underlying reaction mechanisms and optimizing reaction processes, which both are often time-consuming processes.

In situ reaction monitoring may speed up these tasks and can be realized by using Raman spectroscopy since it is sensitive to molecular vibrations and thus reflects the molecules present in the sample. Furthermore, it allows contactless real-time monitoring: the chemical reaction can be measured directly inside a transparent vessel like the usual reaction tube. Therefore, no sample transfer or sample preparation is required. [1]

In addition, Raman spectroscopy may be applied in various chemical environments e.g. in liquid phase [2,3], sol-gel reaction [4], or even in mechanochemical solid-solid reactions in ball mills. [5]

Anton Paar’s Cora Raman spectrometers offer state-of-the-art hardware together with an intuitive software which provides an easy-to-use monitoring mode. Together with a high temperature probe the setup is ideally suited to follow chemical reactions at elevated temperatures.

As a model system for an organic synthesis reaction, this report presents the in situ reaction monitoring of the formation of acetylsalicylic acid, also known as API in aspirin. The synthesis is an example for an acetylation, a basic organic reaction to apply protective groups in organic molecules for multi-step reactions. It introduces an acetyl group by substituting a hydrogen atom for it so that an ester compound is formed.

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