反应详情

To a stirred solution of 2-butyl-2-[(3,4-dichloro-phenyl)-hydroxy-methyl]-pyrrolidine-1-carboxylic acid tert-butyl ester (0.520 g, 1.29 mmol) in DCM (20 mL) at 0° C. under nitrogen was added DMP (0.658 g, 1.55 mmol) in a single portion. The reaction mixture was warmed to ambient temperature and stirred for 30 minutes, then diluted with DCM, washed with 1 N NaOH and brine, then dried (MgSO4), filtered and concentrated in vacuo to a yellow oil (0.62 g). Purification by chromatography (silica, 10-20% EtOAc in hexanes) gave 2-butyl-2-(3,4-dichloro-benzoyl)-pyrrolidine-1-carboxylicacid tert-butyl ester (0.441 g, 1.10 mmol, 85%) as a clear colourless gum.

1. washwashed with 1 N NaOH and brine
2. dry with materialdried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated in vacuo to a yellow oil (0.62 g)
5. customPurification by chromatography (silica, 10-20% EtOAc in hexanes)