Carbon Dioxide → HCID 58379073, compound

Participants

Reaction Steps

Cool methanol (2.82 L) to 0° C. via a 1:1 acetone/water bath with dry ice, and add acetyl chloride (142 mL, 2.0 mol) dropwise over a period of 30 min, maintaining the temperature below 15° C. during the addition. Stir the mixture for 15 min. Add (S)-tert-butyl 4-(4-(4-fluorophenyl)phthalazin-1-yl)-2-methylpiperazine-1-carboxylate (282 g, 667 mmol) in one portion. Stir the mixture for 12 h at 25° C. Concentrate, and dissolve the residue in water (3.0 L). Add solid NaHCO3 until the pH is 7. Extract the product with CH2Cl2 (2×2.0 L), combine the organic layers, and concentrate to give the title compound as a brown crushable foam in quantitative yield (236 g, >100%). ES/MS m/z 323.0 (M+1).

Provenance & Evidence