HCID 54723796, compound → HCID 54723799, compound

Participants

Reaction Steps

HCI (2 N in Et2O, 5 ml) was added dropwise to a stirred solution of tert-butyl 4-hydroxy-9-methyl-2-oxo-1,2,5,6,8,9-hexahydro-7H-pyrido[2,3-d]azepine-7-carboxylate (250 mg, 850 μmol). After 10 h of stirring at room temperature, the reaction was quenched with sat. aq. NaHCO3 and extracted with DCM. The organic layer was dried and concentrated in vacuo to provide 180 mg (92%) of 4-hydroxy-9-methyl-1,5,6,7,8,9-hexahydro-2H-pyrido[2,3-d]azepin-2-one. 1H-NMR (DMSO-d6) δ 13.20 (br s, 2H), 12.93 (br s, 2H), 10.02 (br s, 1H), 9.41 (br s, 1H), 6.65 (s, 1H), 3.51 (br s, 1H), 3.32 (m, 2H), 3.15 (m, 2H), 2.95 (m, 1 H), 2.85 (m, 1 H), 1.39 (d, 3H) ppm.

Provenance & Evidence