Gemini single crystal diffractometer

Unless stated otherwise, reactions were conducted in dried glassware. Commercially available reagents and solvents were used as received. 300–400 mesh silica gel was used for flash column chromatography. Visualization on TLC was achieved by the use of UV light (254 nm). 400 MHz and 100 MHz were used to record the ¹H NMR and ¹³C NMR spectra. Chemical shifts (δ ppm) were reported in parts per million, referring to either the internal standard of TMS or the residue of the deuterated solvents. The splitting pattern was described as follows: s for singlet, d for doublet, t for triplet, q for quartet, and m for multiplet. Coupling constants were reported in Hz. The high-resolution mass spectrum (HRMS) was performed on waters Xevo G2-S QTof mass spectrometer. The crystal of 3k was measured on an Agilent Technologies Gemini single-crystal diffractometer and the solvent system for crystal growth is dichloromethane and petroleum ether.

Unless otherwise stated, all chemical reagents were obtained from commercial suppliers and used without further purification. All of the solvents used were purified and dried by standard methods prior to use.
The ¹H NMR (400 MHz) and ¹³C NMR (100 MHz) spectra were recorded on a Bruker AV III 400 MHz spectrometer with DMSO-d₆ as the solvent and tetramethylsilane (TMS) as an internal reference. UV-Vis absorption spectra were determined on a PERSEE TU-1810 spectrophotometer. FT-IR spectra (400–4000 cm⁻¹) were recorded on a Nicolet 670 spectrometer with a (S/N) of 40 000 : 1 in the solid state (KBr pellets). Single crystal X-ray diffraction (XRD) data were harvested on an Agilent Technologies Gemini single-crystal diffractometer. High resolution mass spectra (HRMS) were carried out on a Shimadzu LCMS-IT-TOF (ESI) spectrometer.