commercial
companies and were used without further purification. Reactions were
monitored by thin-layer chromatography using pre-coated aluminum sheets
(silica gel 60 F254, 0.2 mm thickness). Formation of the
desired product was confirmed by infrared (IR), 1H NMR, 13C NMR, and mass spectra (LC–MS/HRMS). IR spectra were
recorded on a Perkin Elmer Spectrum 400 FTIR instrument, and the frequencies
are expressed in cm–1. 1H NMR and 13C NMR spectra were recorded on a Bruker Avance II-400 spectrometer
in CDCl3, and chemical shifts were recorded in ppm with
TMS as the internal standard. The HMBC spectrum was recorded on an
ECZR series 600 MHz NMR spectrometer (Jeol, Japan). Melting points
were recorded by an open capillary tube method. Mass spectral data
were obtained with a Waters UPLC-TQD mass spectrometer (ESI-MS). High-resolution
mass spectra (ESI-HRMS) were recorded on an Agilent 6545 Quadrupole
Time-of-Flight. All reactions were purified by column chromatography
over silica gel (100–200 mesh) using ethyl acetate and hexane
as the eluent.