Jmn ecz400s

All the reagents and solvents were commercially available and used as received. UV light (310 nm) was irradiated using Techno Sigma LED PER-AMP (Okayama, Japan). The ¹H-NMR spectra were measured on a JEOL JMN-ECZ400S (Tokyo, Japan) at 400 MHz with tetramethylsilane as an internal standard. The ¹³C-NMR spectra were measured on a JEOL JMN-ECZ400S (Tokyo, Japan) at 100 MHz, and assignments of ¹³C-NMR spectra were performed via DEPT experiments. Absorption spectra were recorded on a JASCO V-650 spectrophotometer (Tokyo, Japan). The IR spectra were recorded on a JASCO FT/IR-4200 spectrometer (Tokyo, Japan). The high-resolution mass spectra were measured on an AB SCIEX Triple TOF 4600 (Tokyo, Japan). Diffraction data were collected at 93 K under a cold N₂-gas stream on a Rigaku XtaLAB Synergy-S/Mo system (λ=0.71073 Å (Mo-Kα), Tokyo, Japan). The integrated data were analyzed by using a Yadokari-XG software package [24 (link)]. The structures were solved with the ShelXT structure solution program [25 (link)] using Intrinsic Phasing and refined with the ShelXL refinement package [26 (link)] using least-squares minimization. Anisotropic refinement was performed for all non-hydrogen atoms, and all the hydrogen atoms were put in calculated positions. The geometrical optimization was carried out at the CAM-B3LYP/6-31G(d,p) level of theory implemented on the Gaussian 09 package [27 ].

All reagents were purchased from commercial sources and used without further purification. ¹H and¹³C NMR spectra were recorded on Bruker DPX-400 and JEOL JMN-ECZ400S spectrometers (400 MHz and 100 MHz, respectively) in CDCl₃ using TMS as an internal standard. The assignments of the ¹³C NMR signals were performed by DEPT experiments. IR spectra were recorded on a JASCO FT/IR-4200 spectrometer equipped with an ATR detector. High-resolution mass spectra were obtained on AB SCIEX Triplet TOF 4600 and Bruker Compact mass spectrometers. All measurements were made on a Rigaku AFC7R diffractometer with graphite monochromatized Mo Kα radiation. Melting points were recorded on an SRS-Optimelt automated melting point system and were uncorrected.