反应详情

To a solution of (2S,4S)-1-Boc-4-azidopyrrolidine-2-carboxylic acid (9.5 g, 35 mmol) prepared in Step A in DMF (30□) was added dropwise DIPEA (1.15□, 6.70 mmol), and added dropwise 2M dimethylamine-THF solution (26.3 ml, 52.5 mmol), HOBT (7 g, 52.5 mmol) and EDC (10.2 g, 52.5 mmol) in order. The reaction mixture was stirred at rt for 12 h, and concentrated in vacuo. The residue was diluted with EtOAc, and washed with a saturated NaHCO3 aqueous solution, water and 1N HCl. The organic solution was dried over MgSO4, concentrated in vacuo, and the residue was purified by column chromatography (eluent: EtOAc:Hex=1/2) to give the title compound (9.1 g, 93%).

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