反应详情

Cbz-Dap(Boc)-OH (0.41 g, 1.2 mmol) was treated with a mixture of 1-(3-(dimethylamino)propyl)-3-ethylcarbodiimide methiodide (0.374 g, 1.26 mmol) and N-hydroxybenzotriazole (0.17 g, 1.26 mmol) in N-methylmorpholine (0.28 mL, 2.1 mmol) in dichloromethane. H-Ala-OBn (0.26 g, 1.2 mmol) was added to the above solution and the resulting mixture was stirred for 14 h at room temperature, then diluted with ethyl acetate (40 mL). The organic solution was washed with 10% aqueous citric acid solution (2×30 mL), saturated aqueous sodium bicarbonate solution (2×30 mL) and brine (2×30 mL). The organic layer was dried over magnesium sulfate and then concentrated in vacuo. The crude compound (247) (0.51 g) was used without further purification.

1. washThe organic solution was washed with 10% aqueous citric acid solution (2×30 mL), saturated aqueous sodium bicarbonate solution (2×30 mL) and brine (2×30 mL)
2. dry with materialThe organic layer was dried over magnesium sulfate
3. concentrationconcentrated in vacuo
4. customThe crude compound (247) (0.51 g) was used without further purification