HCID 53705050, compound → HCID 2825090, compound

Participants

Reaction Steps

Methyl 2-diazo-4-methoxy-3-oxobutanoate (4.5 g, 0.026 mol) was cooled in an ice bath and ammonium sulfide (8.0 g, 0.12 mol) (40-48%) was added drop-wise over 2 minutes. White precipitate formed. The slurry was stirred for 30 minutes, and then purified by flash chromatography to give the desired product (4.2 g, 85%) as a light oil, that crystallized readily upon standing. 1H NMR (400 MHz, CD3OD): δ 5.02 (s, 2H), 3.98 (s, 3H), 3.57 (s, 3H). MF═C6H8N2O3S; LCMS calculated for C6H9N2O3S(M+H)+: m/z=189.0.

Provenance & Evidence