反应详情

温度

60 °C

To a solution of 1.5 g (S)-4-carbobenzyloxy-1-(4,5-dichloro-2-nitrophenyl)-piperazine-2-carboxylic acid in 40 mL of acetic acid is added 1.2 g of iron powder. With good stirring, the mixture is heated at 60° C. for 2 hours, then concentrated under reduced pressure (1-2 mm, <40° C.) to a gray-black residue. This material was slurried with 100 mL of ethyl acetate (2×). The combined ethyl acetate filtrates are washed with 100 mL of 1N HCl, 200 mL of water (2×), 100 mL of brine and dried over MgSO4. Filtration and concentration of the solvent gave a semi-solid material that is crystallized from hexane to afford 1.08 g (80.6%) of title compound as a white solid, mp 174-6° C.

1. concentrationconcentrated under reduced pressure (1-2 mm, <40° C.) to a gray-black residue
2. washThe combined ethyl acetate filtrates are washed with 100 mL of 1N HCl, 200 mL of water (2×), 100 mL of brine
3. dry with materialdried over MgSO4
4. filtrationFiltration and concentration of the solvent
5. customgave a semi-solid material that
6. customis crystallized from hexane