Ammonia → HCID 70268047, compound

Participants

Reaction Conditions

Reaction Steps

3,5-Dimethyl-2-hydroxymethyl-4-pyrone 4 (9.75 g, 63.3 mmol) was dissolved in 32% aqueous ammonia (0.880, 60 ml) in a 100 ml round bottom flask. The flask was sealed with a septum cap and made secure with wire. The solution was then stirred at 60° C. for 48 hours before being evaporated to dryness under reduced pressure to give 5 as an off-white solid (9.30 g, 60.8 mmol, 96% yield). Selected IR (cm-1, nujol) 3150-3500 (br, s), 1639 (s); 1H-NMR (DMSO-d6) δ 1.80 (s, 3H), 1.84 (s, 3H), 4.45 (s, 2H), 7.44 (s, 1H); Ms (APCI+) m/z (%) 154 (MH+, 100).

Provenance & Evidence