反应详情

(2S,4S)-1-Boc-4-azidopyrrolidine-2-carboxylic acid (9.5 g, 35 mmol) obtained in Step A was dissolved in DMF (30 mL). After DIPEA (1.15 mL, 6.70 mmol) was added thereto, 1-methylpiperazine (5.81 mL, 52.5 mmol), HOBT (7 g, 52.5 mmol) and EDC (10.2 g, 52.5 mmol) were added thereto, in turn. The reaction solution was stirred for 12 hours at room temperature and concentrated in vacuo. The residue was diluted with EtOAc and washed with saturated NaHCO3 aqueous solution, water and 1N HCl. The extracted organic solution was dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (eluent: MC/MeOH=10/1) to give the title compound (11.67 g, 93%).

1. concentrationconcentrated in vacuo
2. additionThe residue was diluted with EtOAc
3. washwashed with saturated NaHCO3 aqueous solution, water and 1N HCl
4. dry with materialThe extracted organic solution was dried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography (eluent: MC/MeOH=10/1)