Pyridine → HCID 178430146, compound

Participants

Reaction Steps

Compound 12A (30.0 mg, 0.0699 mmol) was dissolved in THF (1 mL) and HF/pyridine (˜2.3:1, 0.075 mL) was added. After stirring at rt overnight, the reaction was concentrated and purified via preparative HPLC (YMC ODS C-18, 21.2×100 mm, eluting with 50-100% solvent B (A=90% H2O-10% MeOH-0.1% TFA and B=10% H2O-90% MeOH-0.1% TFA) over 10 min; Flow rate at 20 mL/min; UV detection at 220 nm. The peaks were collected, combined and repurified via preparative HPLC (YMC ODS C-18, 21.2×100 mm, eluting with 30-100% solvent B (A=90% H2O-10% MeOH-0.1% TFA and B=10% H2O-90% MeOH-0.1% TFA) over 10 min; Flow rate at 20 mL/min; UV detection at 220 nm to provide compound 12B (8.0 mg) as a clear film. MS: m/z 334 [M+H]+.

Provenance & Evidence