Ammonium Acetate → HCID 86671416, compound

Participants

Reaction Steps

A solution of 2-bromo-1-(2-chloropyrimidin-4-yl)ethanone (1.04 mmol, 0.24 g), D6 (1.04 mmol, 0.28 g) and ammonium acetate (4.15 mmol, 0.32 g) in EtOH (20 mL) was stirred at room temperature for 1 hour. The reaction mixture was concentrated. The residue was taken up in water (20 mL) and brought to pH 7 with 5% aqueous NaHCO3. The precipitate was filtered off and purified by flash silicagel chromatography (100% DCM to 10% MeOH) yielding 0.11 g of a yellow solid (26%). 1H-NMR (400 MHz, CDCl3, 300K): δ=1.49 (9H, s), 2.28 (2H, m), 3.55 (6H, m), 5.70 (1H, br s), 7.30 (1H, s), 7.39 (1H, d, J=5.3 Hz), 8.50 (1H, d, J=5.3 Hz), 9.84 (1H, br s); MS (ES) C19H22ClN5O3 requires: 403. found: 404.2 [M+H]+.

Provenance & Evidence