Ammonia → HCID 19771699, compound

Participants

Reaction Steps

Compound C1 (1.0 g) and aqueous ammonia solution (density, 0.91 g/ml; 15 ml) were heated at 120° C. in a sealed tube for 10 hours. Volatile material was removed by evaporation and the residue azeotroped with toluene (2×20 ml). The residue was recrystallised from a mixture of methanol and ethyl acetate to give 2-methyl-1,5,7,8-tetrahydropyrano[4,3-b]-pyridin-4-one (B1) (0.70 g), as an off-white solid, m.p. >285° C.; NMR (d6 -DMSO): 2.2(s,3H), 2.45-2.6(m,2H), 3.8(t,2H), 4.3(t,2H), 5.8(s,1H) 11.1(br s, 1H).

Provenance & Evidence