Upscaling and Risk Evaluation of the Synthesis of the 3,5-Diamino-1H-Pyrazole, Disperazol
Abstract
:1. Introduction
1.1. Safety Assessment of the Active Compound
1.2. Synthetic Route
2. Results and Discussion
2.1. Step 1—Diazotisation
2.2. Step 2—Ring Closure of Pyrazole
2.3. Step 3—Formulation as a Salt
2.4. Summary
3. Materials and Methods
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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TEST | Compound E |
---|---|
Drop-weight impact/Fallhammer (bulk sample) | >100 J |
Friction sensitivity (bulk sample) | >360 N |
Explosion severity, ES; Ignition sensitivity, IS (dust cloud) | Pmax = 9.6 bar (dP/dt)max = 1128 bar/s Kmax = 306 bar·m/s ES = 2.9 IS = 13.1 |
Minimum explosible concentration, MEC (dust cloud) | 50–60 g/m3 Estimate: 56 g/m3 |
Minimum ignition energy, MIE (dust cloud) | 3–10 mJ Estimate: 8 mJ |
Minimum autoignition temperature, MIT (dust cloud) | >600 °C |
Total combustible content (bulk sample) | 100 wt% > 700 °C |
Parameters | Range Tested |
---|---|
Concentration of A | 0.3 M, 0.4 M, 0.6 M, 0.8 M, 1.0 M, 2.0 M |
Temperature | Room temperature (ranging from 23–26 °C), 28 °C, 30 °C |
Coil resident time | 2.5 min, 3 min, 4 min, 5 min, 6.5 min, 7.5 min, 8 min, 10 min, 12 min, 15 min |
Reagents ratio (A:B:TBN) | 1:1:1, 1:1:1.3, 1:1:1.7, 1:1:2, 1:1:2.3, 1:1.1:1, 1:1.2:1, 1:1.3:2, 1:1.3:1.3, 1:1.5:1.3, 1:2:1.3 |
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Jansen, C.U.; Grier, K.E.; Andersen, J.B.; Hultqvist, L.D.; Nilsson, M.; Moser, C.; Graz, M.; Tolker-Nielsen, T.; Givskov, M.; Qvortrup, K. Upscaling and Risk Evaluation of the Synthesis of the 3,5-Diamino-1H-Pyrazole, Disperazol. Int. J. Mol. Sci. 2024, 25, 6737. https://doi.org/10.3390/ijms25126737
Jansen CU, Grier KE, Andersen JB, Hultqvist LD, Nilsson M, Moser C, Graz M, Tolker-Nielsen T, Givskov M, Qvortrup K. Upscaling and Risk Evaluation of the Synthesis of the 3,5-Diamino-1H-Pyrazole, Disperazol. International Journal of Molecular Sciences. 2024; 25(12):6737. https://doi.org/10.3390/ijms25126737
Chicago/Turabian StyleJansen, Charlotte Uldahl, Katja Egeskov Grier, Jens Bo Andersen, Louise Dahl Hultqvist, Martin Nilsson, Claus Moser, Michael Graz, Tim Tolker-Nielsen, Michael Givskov, and Katrine Qvortrup. 2024. "Upscaling and Risk Evaluation of the Synthesis of the 3,5-Diamino-1H-Pyrazole, Disperazol" International Journal of Molecular Sciences 25, no. 12: 6737. https://doi.org/10.3390/ijms25126737