Methanol → HCID 45117257, compound

Participants

Reaction Steps

To a slurry of three combined batches of methyl N-{[(phenylmethyl)oxy]carbonyl}-D-alanyl-N-methylglycinate (combined total 489.09 g, 1586 mmol) in DCM (210 mL) was added MeOH (1000 mL) and 10% Pd/C (50 g). The mixture was hydrogenated at 50 psi overnight, and then an additional portion of 10% Pd/C (5 g) was added. The mixture was hydrogenated at 50 psi for an additional 6 h, and was then filtered and washed with MeOH and DCM. The resulting clear liquid was evaporated to give a clear oil, which subsequently solidified upon standing to afford (3R)-1,3-dimethyl-2,5-piperazinedione (214.0 g, 95% yield) as a pale yellow tinted solid. LCMS: (M+H)+: 143.0.

Provenance & Evidence