Due to the light and air sensitivity of amphotericin B (AmB), all reactions were performed in oven or flame dried glassware under an atmosphere of argon under low light conditions. Compounds were stored under an anaerobic atmosphere. All solvents were dispensed from a solvent purification as described by Pangborn and coworkers51 (THF, Et2O : dry neutral alumina; DMSO, DMF, CH3OH : activated molecular sieves). Triethylamine and pyridine were freshly distilled under nitrogen from CaH2. Camphorsulfonic acid was recrystallized from ethanol. Water was obtained from a Millipore (Billerica, MA) MilliQ water purification system. Reactions were monitored by RP-HPLC using an Agilent 1200 Series HPLC system equipped with an Agilent Zorbax Eclipse C18 3.5-μm, 4.6 × 75 mm column with UV detection at 383 nm at 1.2 mL/min, or an Agilent 6230 ESI TOF LC/MS system equipped with an Agilent Zorbax Eclipse C18 1.8-μm, 2.1 × 50 mm column with UV detection at 383 nm at 0.4 mL/min. Full experimental details and characterization for new compounds appear in the Supplementary Note .
6230 esi tof lc ms system
Manufactured by Agilent Technologies
The 6230 ESI TOF LC/MS system is a high-performance liquid chromatography-mass spectrometry (LC-MS) instrument designed for accurate mass and high-resolution analysis. It utilizes electrospray ionization (ESI) and time-of-flight (TOF) mass spectrometry technology to provide precise and reliable data for a variety of analytical applications.
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2 protocols using 6230 esi tof lc ms system
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Synthesis of Sensitive Amphotericin B
2
Synthesis of Sensitive Amphotericin B
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Due to the light and air sensitivity of amphotericin B (AmB), all reactions were performed in oven or flame dried glassware under an atmosphere of argon under low light conditions. Compounds were stored under an anaerobic atmosphere. All solvents were dispensed from a solvent purification as described by Pangborn and coworkers51 (THF, Et2O : dry neutral alumina; DMSO, DMF, CH3OH : activated molecular sieves). Triethylamine and pyridine were freshly distilled under nitrogen from CaH2. Camphorsulfonic acid was recrystallized from ethanol. Water was obtained from a Millipore (Billerica, MA) MilliQ water purification system. Reactions were monitored by RP-HPLC using an Agilent 1200 Series HPLC system equipped with an Agilent Zorbax Eclipse C18 3.5-μm, 4.6 × 75 mm column with UV detection at 383 nm at 1.2 mL/min, or an Agilent 6230 ESI TOF LC/MS system equipped with an Agilent Zorbax Eclipse C18 1.8-μm, 2.1 × 50 mm column with UV detection at 383 nm at 0.4 mL/min. Full experimental details and characterization for new compounds appear in the Supplementary Note .
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