Jms gcmate mass spectrometer

For specific rotation, a Horiba SEPA-300 digital polarimeter (5 cm) was used and IR data was collected from a Shimadzu FTIR-8100 spectrometer. For mass spectrometry measurements, IMS was performed on a Finnegan LCQ ion trap mass spectrometer and HR-EI-MS experiments were performed on Fourier transform ion cyclotron mass spectrometer. EI-MS experiments were performed a JEOL JMS-GCMATE mass spectrometer. Using tetramethylsilane as an internal standard, the ¹H (600 MHz) and ¹³C (150 MHz) NMR spectra were achieved on a JEOL JNM-ECA 600 spectrometer. Compound separation for analytical and preparative separation was carried out using YMC-Pack ODS-A (250 × 4.6 mm i.d.) and (250 × 20 mm i.d.) columns, respectively. Purification was performed using a Shimadzu HPLC system furnished with a RID-10A refractive index detector. Fuji Silysia Chemical, Ltd.'s normal-phase silica BW-200 (Fuji Silysia Chemical, Ltd., 150–350 mesh) and Chromatorex's ODS reverse phase DM1020T (Fuji Silysia Chemical, Ltd., 100–200 mesh) were used for chromatography separations (Fuji Silysia Chemical, Ltd., 100–200 mesh). Additionally, silica gel 60 F₂₅₄ (Merck, 0.25 mm) and RP-18 WF₂₅₄ were used (Merck, 0.25 mm) for TLC analysis with compound visualization by with H₂SO₄–MeOH (1 : 9) spray followed by heating.