Mercury 400 100 mhz spectrometer

Reagents were used as purchased without further purification. Solvents (dichloromethane, methanol, acetonitrile, toluene, ethanol, ethyl acetate) were dried and stored using molecular sieves. TLC was performed on precoated silica gel polyester plates (0.25 mm thickness) through the use of a UV fluorescence indicator 254 (Polychrom SI F254). Chromatographic separations were performed on silica gel columns via flash (Kieselgel 40, 0.040–0.063 mm; Merck, Rahway, NJ, USA) chromatography. The compound/stationary phase ratio was 1g of compound/50 g of silica gel. ¹H NMR and ¹³C NMR spectra were recorded in CDCl₃, CD₃OD, DMSO-d₆, or C₃D₆O using a Bruker SY spectrometer at 400/100 MHz or a Varian Mercury 400/100 MHz spectrometer. DEPT-135 and DEPT-90 spectra were recorded to identify the C, CH, CH₂, and CH₃ signals (Figures S1–S16 in Supplementary Materials). Chemical shifts (δ) are given in ppm downfield from tetramethylsilane, and coupling constants (J values) are given in Hz. IR spectra in KBr disks were run on a Nicolet Impact 410 Spectrophotometer (see Figures S17–S32 in Supplementary Materials). A hybrid QSTAR XL quadrupole/time of flight spectrometer was used for HRMS analyses. The aqueous solubility of the compounds was determined in a Helios Alfa Spectrophotometer from Thermo-Spectronic.

Reagents were used as purchased without further purification. Solvents (toluene, ethanol, EtOAc, CH₂Cl₂, MeOH) were dried and stored over molecular sieves. TLC was performed on precoated silica gel polyester plates (0.25 mm thickness) with a UV fluorescence indicator 254 (Polychrom SI F254). Chromatographic separations were performed on silica gel columns via flash (Kieselgel 40, 0.040–0.063; Merck, Rahway, NJ, USA) chromatography. ¹H NMR and ¹³C NMR spectra were recorded in CDCl₃, CD₃OD, DMSO-d₆, or acetone-d₆ on a Bruker SY spectrometer at 400/100 MHz or on a Varian Mercury 400/100 MHz spectrometer. Chemical shifts (δ) are given in ppm downfield from tetramethylsilane, and coupling constants (J values) are given in Hz. IR spectra in KBr disks were run on a Nicolet Impact 410 Spectrophotometer. A hybrid QSTAR XL quadrupole/time of flight spectrometer was used for HRMS analyses. The aqueous solubility of the compounds was determined in a Helios Alfa Spectrophotometer from Thermo-Spectronic.