Cms l compact mass spectrometer

The purity of all final compounds was >95 % purity as assessed by HPLC. Final compounds were analyzed on an Agilent 1200 series chromatograph. The chromatographic method utilized as ThermoScientific Hypersil GOLD C-18 4.6 × 250 mm, 3 μm column. UV detection wavelength = 220 nm; flow-rate = 1.0 mL/min; gradient = 5 - 95% acetonitrile over 12 min and 3 min hold time at 95% acetonitrile. Both organic and aqueous mobile phases contain 0.1% v/v formic acid. The mass spectrometer used is an AB Sciex 4500 QTrap triple-quadrupole mass spectrometer with an ESI source or an Advion CMS-L Compact Mass Spectrometer with an ESI or an APCI source. Samples are submitted for analysis solubilized in 1:1 acetonitrile:water solution or using the atmospheric solids analysis probe (ASAP). ¹H and ¹³C NMR spectra were recorded on either Bruker DRX500 spectrometer (operating at 500 and 125 MHz, respectively) or Bruker AVIII (operating at 800 and 200 MHz, respectively) in DMSO-d₆ or CDCl₃ with or without the internal standard of TMS at 0.05% v/v. The chemical shifts (δ) reported as parts per million (ppm) and the coupling constants are reported as s = singlet, bs = broad singlet, d = doublet, t = triplet, q = quartet, dd = doublet of doublet, m = multiplet. Compounds were generally prepared according to scheme 1 and protocols are detailed below. Intermediate 4C was commercially available.

The purity of all final compounds was ascertained via HPLC on an Agilent 1200 series chromatograph >95%. Chromatographic methods utilized include a ThermoScientific Hypersil GOLD C-18 4.5 × 250 mm, 3 μm column, UV detection at a wavelength of 254 nm, flow rate set to 1.0 mL/min, and with an acetonitrile: water gradient from 5 to 95% acetonitrile over 12 min with a 3 min hold time at 95%. Both acetonitrile and water contained 0.1% v/v formic acid. Mass spectrometry was obtained on an Advion CMS-L Compact Mass Spectrometer with an atmospheric pressure chemical ionization (APCI) or electrospray ionization (ESI) source on normal or low fragmentation settings. ¹H and ¹³C NMR spectra were recorded on either a Bruker DRX500 spectrometer or a Bruker AVIII in CDCl₃, DMSO-d₆, or methanol-d₄ with the internal standard of TMS at 0.05% v/v. Chemical shifts (δ) reported below are as parts per million (ppm) and the coupling constants are reported as follows: s = singlet, d = doublet, t = triplet, q = quartet, p = pentet, h = hextet, hept = heptet, dd = doublet of doublets, ddd = doublet of doublet of doublets, and m = multiplet. Protocols for each compound are detailed below. Compounds were prepared according to Scheme 1 and a protocol is detailed below for compound 1. All other compound synthesis and characterization data are provided in the Supporting Information.

¹H and ¹³C NMR spectra were recorded on Bruker DRX500 spectrometer (operating at 500 and 126 MHz) in DMSO-d₆ or CDCL₃ with or without the internal standard of TMS at 0.05% v/v. The chemical shifts (d) reported as parts per million (ppm) and the coupling constants are reported as s = singlet, bs = broad singlet, d = doublet, t = triplet, q = quartet, dd = doublet of doublet, m = multiplet. The purity of all final compounds was >95 % purity as assessed by HPLC according to current American Chemical Society guidelines for publication. Final compounds were analyzed on an Agilent 1200 series chromatograph. The chromatographic method utilized as ThermoScientific Hypersil GOLD C-18 or silica column. UV detection wavelength = 220/254 nm; flow-rate = 1.0 mL/min; solvent = acetonitrile/water for reverse phase. Both organic and aqueous mobile phases contain 0.1% v/v formic acid. The mass spectrometer used is an Advion CMS-L Compact Mass Spectrometer with an ESI or an APCI source. Samples are submitted for analysis using the atmospheric solids analysis probe (ASAP). Compounds were prepared according to following protocols and are detailed below.