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Updated: Feb 20, 2026

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy
Published on: October 9, 2020
Mechanochemical Knoevenagel condensation investigated in situ
Sebastian Haferkamp1,2, Franziska Fischer1, Werner Kraus1
1BAM Federal Institute for Materials Research and Testing, Richard-Willstaetter-Str. 11, 12489 Berlin, Germany.
Abstract:
The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.
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