by an open capillary using a Veego precision digital melting point
apparatus (MP-D) and are uncorrected. 1H NMR spectra were
recorded in CDCl3 with a Bruker AVANCE II (500 MHz) spectrometer
using tetramethylsilane (TMS) as the internal standard. Chemical shift
values are expressed as parts per million downfield from TMS, and
the J values are in hertz. Splitting patterns are
indicated as s: singlet, d: doublet, t: triplet, m: multiplet, dd:
double doublet, ddd: doublet of a doublet of a doublet, and br: broad
peak. 13C NMR spectra were recorded in CDCl3 with a Bruker AVANCE II (125 MHz) spectrometer using TMS as the
internal standard. Mass spectra were recorded on a Bruker high resolution
mass spectrometer (micrOTOF-QII). Elemental analyses were performed
on a Heraeus CHN-O-Rapid elemental analyzer.20e Column chromatography
was performed on a silica gel (60–120 mesh) using an ethyl
chloroform/hexane mixture as the eluent.