Rt dr bf 1h 5 mm oz smartprobe

1D and 2D NMR experiments were recorded on Bruker Avance NEO 400 MHz and 700 MHz spectrometers (Bruker, USA) with a RT-DR-BF/1H-5mm-OZ SmartProbe. Chemical shifts were reported in δ (ppm) and were referenced to the residual CDCl₃ as internal standards (δ_H = 7.26 and δ_C = 77.0 ppm) and CD₃OD as internal standards (δ_H = 3.31 e δ_C = 49.0 ppm). All of the recorded signals were in accordance with the proposed structures. Spin multiplicities are given as s (singlet), br s (broad singlet), d (doublet), t (triplet) or m (multiplet).
The LC-HRMS and MS/MS analysis were carried out on an LTQ XL-Orbitrap high-resolution mass spectrometry system (Thermo Scientific) equipped with an Accelera 600 pump HPLC (LCHRMS).
Further fragmentation analysis was carried out on an LTQ XL mass spectrometry system (Thermo Scientific) equipped with a HESI source and connected to an Ultimate 3000 HPLC pump.
The first purification step was run on a User Manual PuriFlash XS 520 Plus equipped with UV detector. Purification of single molecules was performed on an Acquity UPLC H-CLASS connected to a PDA detector (Waters).
The 96-well plates were read on a Biotek ELX800, monitoring the absorbance at 600 nm at room temperature.

Electrospray ionization mass spectrometry (ESI-MS) experiments were performed on an Applied Biosystem API 2000 triple-quadrupole mass spectrometer. Optical rotations were determined on a Jasko P-2000 polarimeter. Nuclear magnetic resonance (NMR) spectra were recorded on a Bruker Avance NEO 400 spectrometer equipped with an RT-DR-BF/1H-5 mm-OZ SmartProbe (¹H at 400 MHz and ¹³C at 100 MHz), δ (ppm), J in Hz, using a solvent signal for the calibration (¹³CD₃OD at δ_C 49.0 and residual CD₂HOD at δ_H = 3.31). The heteronuclear single quantum coherence (HSQC) spectra were optimized for an average ¹J_CH of 140 Hz; the gradient-enhanced heteronuclear multiple bond correlation (HMBC) experiments were optimized for a ³J_CH of 8 Hz. Droplet counter-current chromatography (DCCC) fractionation was performed on DCC-A apparatus (Tokyo Rikakikai Co., Tokyo, Japan) equipped with 250 glass-columns. High-performance liquid chromatography (HPLC) was performed using a Waters 510 pump equipped with a Rheodyne 7125 injector and a Waters 401 differential refractometer as the detector on a C₁₈ μ-Bondapak column (30 cm × 3.9 mm i.d) (Waters, Milford, MA, USA).

HRMS data were acquired in positive mode using a Thermo LTQ Orbitrap XL mass spectrometer (Thermo Fisher Scientific Inc., Waltham, MA, USA) linked to a Thermo U3000.
NMR spectra were recorded on Bruker Avance NEO 400 spectrometer equipped with a RT-DR-BF/1H-5 mm-OZ SmartProbe. Coupling constants (J) are given in Hertz (Hz), chemical shifts were given in δ (ppm) and were referred to the residual CHCl₃ as the internal standard (δ_H = 7.26). Spin multiplicities are given as s (singlet), br s (broad singlet), d (doublet).