Ammonia → HCID 58932541, compound

Participants

Reaction Conditions

Reaction Steps

1′-(3-Aminopropyl)-5′-fluorospiro[1,3-dioxane-2,3′-indol]-2′(1′H)-one (2.37 g, 8.46 mmol) was dissolved in 2M EtOH.NH3 (200 mL), poured into a steel pressure vessel, and heated at 135° C. for 46 hr. The reaction mixture was cooled to room temperature and concentrated. The crude product was purified on Biotage KP silica gel eluting with CH2Cl2/CH3OH/NH4OH (97/2/1) followed by a second chromatography eluting with 80/20 Pet ether/acetone to give the title compound as a white solid (1.52 g, 68% yield). Anal. Calc'd for C14H15FN2O2: C, 64.11; H, 5.76; N, 10.68. Found: C, 64.05; H, 5.79; N, 10.61. NMR (300 Mz, DMSO-d6): consistent; MS: (APCI+) m/z 263 [M+H]. m.p.: 130-132° C.

Provenance & Evidence