Water → HCID 178439942, compound

Participants

Reaction Steps

The material prepared in Step E (160 mg, 0.24 mmol) was dissolved in glacial HOAc (2.0 mL) at 50° C. and H2O was added dropwise until the solution just became cloudy (approx. 0.7 mL). The mixture was kept at 50° C. for 2 hours and then was evaporated to dryness under a stream of nitrogen. The residue so formed was purified by preparative tlc on 1000μ SiO2 plates developed with CHCl3 /MeOH/NH4OH (80:20:2) to give 67 mg (68%) of the title compound as its ammonium salt. 1H NMR (200 MHz, DMSO-d6)δ 6.82-7.80 (m), 5.21 (s), 3.66 (s), 2.70 (t, J=9 Hz), 1.93 (s), 1.52-1.76 (m), 0.89 (t, J=9 Hz). FAB-MS: 413 (M+ +1). Anal. Calcd for C23H24N8 ·NH3 ·0.6 H2O; C, 62.74; H, 6.46; N, 28.63; Found: C, 62.49; H, 6.24; N, 28.73.

Provenance & Evidence