反应详情

温度

50 °C

A 500-mL round-bottomed flask was charged with di-tert-butyl (2R)-2-((1-methylethyl)carbamoyl)-1,4-piperazinedicarboxylate (1.77 g, 4.76 mmol, step 1), BH3.THF (1.0 M in THF, 15.0 mL, 15.0 mmol) and THF (60 mL). The mixture was heated at 50° C. for 12 h. After allowing the reaction to cool to room temperature, additional BH3.THF (1.0 M in THF, 5.0 mL, 5.0 mmol) was added. The mixture was then heated at 50° C. for 1.5 h. The reaction mixture was allowed to cool to room temperature and MeOH (20 mL) was slowly added. The solvent was removed in vacuo and the crude product was purified by column chromatography (100 g of silica gel, 0 to 10% iPrOH (with 10% NH4OH) in CHCl3) to afford di-tert-butyl (2S)-2-(((1-methylethyl)amino)methyl)-1,4-piperazinedicarboxylate (0.69 g) as a clear oil.

1. customthe reaction
2. temperatureto cool to room temperature
3. temperatureThe mixture was then heated at 50° C. for 1.5 h
4. temperatureto cool to room temperature
5. customThe solvent was removed in vacuo
6. customthe crude product was purified by column chromatography (100 g of silica gel, 0 to 10% iPrOH (with 10% NH4OH) in CHCl3)