Sodium Chloride → HCID 18444338, compound

Participants

Reaction Steps

O-Benzotriazol-1-yl-N,N,N′N′-tetramethyluronium tetrafluoroborate (0.108 g, 0.34 mmol) and diisopropylethylamine (0.074 g, 0.57 mmol) were added sequentially at ambient temperature to a stirred solution of N-[2-fluoro-5-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)phenylcarbamoylmethyl]-N-methylglycine (0.103 g, 0.26 mmol) in dimethylacetamide (1 ml), the mixture was stirred at ambient temperature for 1 hour, then it was diluted with water (10 ml). Sodium chloride (1 g) was added, the mixture was stirred at ambient temperature for 30 minutes, then the resulting solid was collected by filtration, washed with water (1 ml) and dried in vacuo to give 1-[2-fluoro-5-(4-oxo-3,4-dihydrophthalazin-1-ylmethyl)phenyl]-4-methylpiperazine-2,6-dione (0.071 g) as a beige solid, m.pt. 205–208° C.; 250 MHz 1H-nmr (CDCl3) δ (ppm): 2.4 (s, 3H) (CH3), 3.5 (q, 4H) (2×CH2), 4.25 (s, 2H) (ArCH2—), 7.1 (m, 2H) (2×ArH), 7.25 (m, 1H) (ArH), 7.7–7.85 (m, 3H) (3×ArH), 8.4 (m, 1H) (ArH), 10.35 (s, 1H) (CONH); m/z (M+H)+. 381, 100% purity.

Provenance & Evidence