O-Methylhydroxylamine hydrochloride → HCID 178449944, compound

Participants

Reaction Steps

To a solution of 2-{(2-chlorophenyl)[(3-methylbutan-2-yl)amino]methylene}-3-oxohexanenitrile (0.300 g, 0.919 mmol, 1 eq.) in ethanol (6 ml) were added methoxylamine hydrochloride (0.314 g, 3.67 mmol, 4 eq.) followed by 2 drops of concentrated sulfuric acid. The reaction was microwaved (150° C., 22000 s, fixed hold, high absorption) and the solvent evaporated. The residual oil was triturated in ethyl acetate and washed with sat. aq. solution of NaCl. After drying over MgSO4 and concentration under vacuum, the residual oil was subjected to preparative HPLC to give 2-{(2-chlorophenyl)[(3-methylbutan-2-yl)amino]methylene}-3-(methoxyimino)hexanenitrile (0.163 g, 49% yield).

Provenance & Evidence