6120 quadrupolems detector

All solvents
were reagent grade or HPLC grade.
Unless otherwise noted, all materials were obtained from commercial
suppliers and used without further purification. All reactions were
performed under nitrogen. Melting points were obtained on a Mel-Temp
apparatus and are uncorrected. ¹H NMR spectra were recorded
at 400 MHz. ¹³C NMR spectra were recorded at 100 MHz. The
HPLC solvent system consisted of distilled water and acetonitrile,
both containing 0.1% formic acid. Preparative HPLC purification was
performed on an Agilent 1200 series HPLC system equipped with an Agilent
G1315D DAD detector using a Phenomenex Luna 5 μm C18 (2) column
(21.2 mm × 250 mm, 5 μm). Analytical HPLC was performed
on an Agilent 1200 series HPLC system equipped with an Agilent G1315D
DAD detector (detection at 220 nm) and an Agilent 6120 quadrupole
MS detector. Unless otherwise specified, the analytical HPLC conditions
involve a gradient of 20% acetonitrile/80% water for 0.5 min followed
by an increase to 85% acetonitrile/15% water over 4 min and continuation
of 85% acetonitrile/15% water for 3.5 min with a Luna C18 column (2.1
mm × 50 mm, 3.5 μm) at a flow rate of 0.75 mL/min. All
final compounds tested were confirmed to be of ≥95% purity
by the HPLC methods described above. The model of compound 11h bound to human DAAO (Figure 4) was generated using AutoDock Vina.^{30 (link)}