2-(4-Nitrobenzylidene)malononitrile

Chang, Min; Fang, Tzu-Chien; Tsai, Hsing-Yang; Luo, Ming; Chen, Kew‐Yu

doi:10.1107/s1600536812008896

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2017

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“…The XRPD patterns of the product for both types of experiments are comparable and the crystals obtained in the in situ reactions are of sufficient quality for X-ray single crystal determination. The crystal structure could be solved, matching the parameters described in the literature [26]. …”

Section: Resultsmentioning

confidence: 99%

Mechanochemical Knoevenagel condensation investigated in situ

Haferkamp

Fischer

Kraus

et al. 2017

Beilstein J. Org. Chem.

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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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Section: Resultsmentioning

confidence: 99%