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Mechanochemistry paves the way to simple, fast, and green syntheses. Despite considerable effort, there is a lack in understanding of the underlying mechanisms. In situ investigations help to understand these mechanisms, which occur during a mechanochemical reaction. Here we present a universal strategy for simultaneous real-time in situ analysis, combining X-ray diffraction, Raman spectroscopy, and thermography. The potential of of our approach is shown for diffrent model reactions.
Studies on the mechanochemical Knoevenagel condensation of fluorinated benzaldehyde derivates
(2018)
The mechanochemical Knoevenagel condensation of three fluorinated benzaldehyde derivates and malononitrile was investigated. The reactions were performed under solvent- and catalyst-free conditions and resulted in highly crystalline products after crystallization from a viscous phase in the milling jar.
The quality of the obtained crystals was sufficient for single-crystal X-ray diffraction circumventing a recrystallization step. To gain more information on the reaction, progress was investigated in situ using time-resolved Raman spectroscopy. The results show a direct conversion of the reactants.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.
Mechanaochemistry is an effective method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of
mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.
Mechanaochemistry is an effecthive method to yield pure compounds within a short reaction time. Mechanochemical C-C bond forming reactions gained increasing interest in the past decade. Among those the Knoevenagel condensation is an important reaction for synthezing a,b-unsaturated compounds. The information on the underlying mechanisms of mechanochemical reactions are scarce. In situ investigations using Raman spectroscopy and synchroton XRD either alone or in combination address this challenge. We present the in situ results of a Knoevenagel condensation with p-nitrobenzaldehyde and malononitrile under neat grinding conditions.