反应详情

To a solution of 3-amino-1-benzyl-4-methylpyrrolidine (9.5 g) in methanol (190 ml) is added anhydrous t-butoxycarboxylic acid (13.0 g) at room temperature, and the mixture is stirred for one hour. Methanol is distilled off under reduced pressure, and to the resulting residue is added water. The mixture is extracted with dichloromethane, and the extract is dried over magnesium sulfate and then dichloromethane is distilled off. The residue is purified by silica gel column chromatography (solvent, dichloromethane:methanol=19:1) to give 3-(t-butoxycarbonylamino)-1-benzyl-4-methylpyrrolidine (isomer A) (4.4 g), as colorless prisms, m.p. 131.5°-132.7° C.

1. distillationMethanol is distilled off under reduced pressure
2. additionto the resulting residue is added water
3. extractionThe mixture is extracted with dichloromethane
4. dry with materialthe extract is dried over magnesium sulfate
5. distillationdichloromethane is distilled off
6. customThe residue is purified by silica gel column chromatography (solvent, dichloromethane:methanol=19:1)