反应详情

温度

0 °C

2-{4-[2-Amino-3-(4-chlorophenyl)-propionyl]-3-ethyl-piperazin-1-yl}-N-methyl-3-naphthalen-2-yl-propioamide HCl, 45, (0.5 g, 0.7 mmol) and Boc-L-proline (0.17 g, 0.78 mmol), 1-(3-dimethylamino-propyl)-3-ethylcarbodiimide (0.19 g, 1.4 mmol) and 1-hydroxybenzotriazole (0.16 g, 0.86 mmol) are dissolved in anhydrous DMF (2.5 mL). The reaction mixture is cooled to 0° C., then N-methylmorpholine (0.6 mL, 5.3 mmol) is added. This reaction mixture is placed in a refrigerator overnight. EtOAc (25 mL) and water (75 mL) are added, and the organic layer is separated. The aqueous layer is extracted with EtOAc (3×30 mL). All organic layers are combined and washed with water (2×50 mL), and dried over Na2SO4. Solvent is removed in vacuo to afford 0.5 g of the desired product.

1. customis placed in a refrigerator overnight
2. customthe organic layer is separated
3. extractionThe aqueous layer is extracted with EtOAc (3×30 mL)
4. washwashed with water (2×50 mL)
5. dry with materialdried over Na2SO4
6. customSolvent is removed in vacuo