Ethanol → HCID 178508576, compound

Participants

Reaction Steps

5-Fluoro-6-chloro-2,4-pyrimidinediamine, 3-oxide (6) (58 mg, 0.32 mmol), piperidine (112 mg, 1.3 mmol) and 95% ethanol (2.6 ml) were charged to a round bottom flask and refluxed for 2 days. The solution was concentrated and the residue was chromatographed on silica gel (elution with 15% methanol/chloroform+2% ammonium hydroxide), yielding 5fluoro-6-piperidinyl-2,4-pyrimidinediamine 3-oxide as a white solid. (51 mg, 69%): MS (70 eV, EI)m/z (relative intensity) 84 (100), 227 (M+, 98), 210 (55), 43 (30), 40 (24); 1H NMR (CD3OD)δ4.91 (s, 4H), 3.61 (mult., 4H), 1.67 (mult., 2H), 1.60 (mult., 4H); 13C NMR (CD3OD) ppm 150, 147.5, 147, 123, 49.86, 27.05, 25.82. Exact Mass Calcd for C9H4N5OF: 227.1182. Found: 227.1188. ##STR2##

Provenance & Evidence