HCID 18401472, compound → HCID 18401479, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of crude 1-(chloromethyl)-4-ethyl-piperazine-2,3-dione (170 mg, 0.9 mmol) in CDCl3 (1 ml) solid potassium thioacetate (123 mg, 1.08 mmol) was added with stirring at 0° C. The reaction mixxture was allowed to stir at room temperature overnight. The mixture was centifuged and the supernatant solution collected. The residual solid (KCl) was washed with CDCl3 (2 ml) and the organic solutions combined and the solvent removed in vacuo. The residue was chromatographed on silica gel (6 g, 63-200 μm) using chloroform-methanol (19:1) to give 1-(acetylthiomethyl)-4- ethyl-piperazine-2,3-dione as a white solid (overall yield 44%). NMR-specrum in CDCl3: 1.22 (t, 3H, J=7 Hz), 2.44 (s, 3H), 3.48 (q, 2H, J=7 Hz), 3.4-3.7 (m, 4H), 4.95 (s, 2H) ppm.

Provenance & Evidence