Gomes Carla, Vinagreiro Carolina S, Damas Liliana, Aquino Gilberto, Quaresma Joana, Chaves Cristina, Pimenta João, Campos José, Pereira Mariette, Pineiro Marta
University of Coimbra, CQC, Department of Chemistry, Rua Larga, 3004-535 Coimbra, Portugal.
Faculty of Pharmacy, Exact Sciences and Technology Unit, State University of Goias, 75132400 Anapolis, Goias, Brazil.
ACS Omega. 2020 May 8;5(19):10868-10877. doi: 10.1021/acsomega.0c00521. eCollection 2020 May 19.
Mechanochemistry is an alternative for sustainable solvent-free processes that has taken the big step to become, in the near future, a useful synthetic method for academia and the fine chemical industry. The apparatus available, based on ball milling systems possessing several optimizable variables, requires too many control and optimization experiments to ensure reproducibility, which has limited its widespread utilization so far. Herein, we describe the development of an automatic mechanochemical single-screw device consisting of an electrical motor, a drill, and a drill chamber. The applicability and versatility of the new device are demonstrated by the implementation of di- and multicomponent chemical reactions with high reproducibility, using mechanical action exclusively. As examples, chalcones, dihydropyrimidinones, dihydropyrimidinethiones, pyrazoline, and porphyrins, were synthesized with high yields. The unprecedented sustainability is demonstrated by comparison of EcoScale and -factor values of these processes with those previously described in the literature.
机械化学是可持续无溶剂工艺的一种替代方法，在不久的将来，它已迈出了重要一步，成为学术界和精细化工行业有用的合成方法。现有的基于具有多个可优化变量的球磨系统的设备，需要进行太多的控制和优化实验以确保可重复性，这限制了其迄今为止的广泛应用。在此，我们描述了一种由电动机、钻头和钻腔组成的自动机械化学单螺杆装置的开发。通过仅使用机械作用实现具有高重现性的二元和多组分化学反应，证明了新装置的适用性和多功能性。例如，以高产率合成了查耳酮、二氢嘧啶酮、二氢嘧啶硫酮、吡唑啉和卟啉。通过将这些工艺的生态规模和E因子值与文献中先前描述的值进行比较，证明了前所未有的可持续性。
