2026-10-14T09:47:50Z https://api.figshare.com/v2/oai

oai:figshare.com:article/34030500 2026-09-30T07:16:35Z category_1 category_4 category_146 category_7 category_14 category_21 category_873 portal_63 item_type_6 month_year_09_2026

A Novel Integrated Microwave/UV/In Situ Fourier Transform Infrared Platform: Application to 1,5-Benzodiazepines Synthesis Alina Cherniienko (25142343) Kacper Kossakowski (25142346) Lucjusz Zaprutko (745302) Roman Lesyk (779012) Anna Pawełczyk (21262955) Biophysics Biochemistry Space Science Medicine Molecular Biology Biotechnology Chemical Sciences not elsewhere classified unprecedented instrumental triad physical catalyst limitations mode thermal heating mapping kinetic bottlenecks ideal catalytic conditions highly tunable paradigm high design flexibility functional group transformations dynamic spectral shift discrete offline sampling conventional “ black box ” trial achieving isolated yields 3 mol %) highly optimized synthesis otf )< sub novel integrated microwave 3 </ sub </ sub simultaneous microwave novel integration ultraviolet dual triflate ν transform infrared synergistic mw study introduces solvent effects scientific research rapid preparation mw ), multimodal platform molecular iodine model condensation error strategies diverse areas benzodiazepines synthesis aromatic diamine apparatus approach The real-time monitoring and optimization of synthesis remain significantly limited by conventional “black-box” trial-and-error strategies. This study introduces an unprecedented instrumental triad: the novel integration of quantitative real-time, in situ attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy with simultaneous microwave (MW), and ultraviolet dual-activation. We deployed this multimodal platform to engineer an evidence-based, highly optimized synthesis of 1,5-benzodiazepines. Rather than relying on discrete offline sampling, continuous spectral tracking enabled rapid identification of ideal catalytic conditions, highlighting the green Lewis acid Sc(OTf)₃ (3 mol %) and molecular iodine (5 mol %) across diverse solvent environments. Crucially, the synergistic MW + UV dual-activation fundamentally outperformed single-mode thermal heating. In the model condensation of aromatic diamine and acetone, this physical synergy accelerated reaction completion to just 4.5 and 8.5 min, achieving isolated yields of 97 and 93% for Sc(OTf)₃ and I₂, respectively. Furthermore, the incorporation of time-resolved ATR-FTIR coupled with standard addition protocols enabled precise quantitative tracking of functional group transformations and provided direct empirical evidence of catalyst–substrate coordination, as demonstrated by the dynamic spectral shift of the triflate ν_sSO₃ band. By mapping kinetic bottlenecks, solvent effects, and physical catalyst limitations, this novel multimodal approach offers a powerful, sustainable, and highly tunable paradigm for the rapid preparation of pharmacologically relevant nitrogen heterocycles. Moreover, this apparatus approach is characterized by high design flexibility, enabling its further modification and adaptation to diverse areas of scientific research. 2026-09-30T00:00:00Z Text Journal contribution 10.1021/acsomega.6c07314.s001 https://figshare.com/articles/journal_contribution/A_Novel_Integrated_Microwave_UV_In_Situ_Fourier_Transform_Infrared_Platform_Application_to_1_5-Benzodiazepines_Synthesis/34030500 CC BY-NC 4.0