Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 76171765, compound

Participants

Reaction Steps

N,O-Dimethylhydroxylamine hydrochloride (0.067 g, 0.3 mmol) was added to a room temperature solution of 3-(4-Formyl-phenyl)-4-hydroxy-6-oxo-3a,6,7,7a-tetrahydro-thieno[2,3-b]pyridine-5-carbonitrile (0.1 g, 0.29 mmol) and sodium acetate (0.025 g, 0.3 mmol) in 1:1:1 mixture of methanoldioxane/water (6 mL). The reaction mixture was quenched with 3N HCl after complete reaction, extracted with ethyl acetate (3×20 mL), organic extracts washed with brine, dried (MgSO4) and concentrated to a brown solid. MS (ESI) m/e 369.5 (M+H)+; 1H NMR (300 MHz, DMSO-d6): δ ppm 12.30 (br s, 1H), 8.36 (s, 1H), 7.59 (d, J=9, 2H), 7.47 (d, J=9, 2H), 7.03 (s, 1H), 4.66 (s, 2H).

Provenance & Evidence