NMR spectra were recorded using the Varian spectrometers
Gemini 2000 or
Unity 500 (Varian GmbH, Darmstadt, Germany) δ given in ppm,
J in Hz; typical experiments: APT, H-H-COSY, HMBC, HSQC, NOESY), MS spectra were taken on a Finnigan MAT LCQ 7000 (ThermoFisher Scientific, Braunschweig, Germany) electrospray, voltage 4.1 kV, sheath gas nitrogen) instrument. The optical rotations were measured on a Perkin-Elmer polarimeter (Perkin Elmer LAS, Rodgau, Germany) or on a Jasco P-2000 polarimeter (Jasco Germany, Pfungstadt, Germany) at 20 °C; TLC was performed on NP or RP18 silica gel (Macherey-Nagel, detection with cerium molybdate or Dragendorff’s reagent). Melting points are uncorrected (
Leica hot stage microscope, or BUCHI melting point M-565), and elemental analyses were performed on a Foss-Heraeus
Vario EL (CHNS, Elementar Analysensysteme GmbH, Langenselbold, Germany) unit. IR spectra were recorded on a Perkin Elmer
FT-IR spectrometer Spectrum 1000 or on a
Perkin-Elmer Spectrum Two (UATR Two Unit; both instruments from Perkin Elmer LAS, Rodgau, Germany). UV-VIS spectra were taken on a Perkin-Elmer Lambda 14 spectrometer or on a Perkin-Elmer Lambda 750 S (UV/VIS/NIR) spectrometer (both instruments from Perkin Elmer LAS, Rodgau, Germany). The solvents were dried according to usual procedures. The purity of the compounds was determined by HPLC and found to be >96%.
Kahnt M., Hoenke S., Fischer L., Al-Harrasi A, & Csuk R. (2019). Synthesis and Cytotoxicity Evaluation of DOTA-Conjugates of Ursolic Acid. Molecules, 24(12), 2254.