反应详情

A mixture of K2CO3 (7.9 g, 57.4 mmol) and diethyl 1H-indole-2,6-dicarboxylate (Intermediate A, 5.0 g, 19.1 mmol) in DMF (30 mL) is stirred at room temperature for 30 min. A solution of 2-bromo-propionitrile (3.4 mL, 38.3 mmol) in DMF (10 mL) is added. The reaction mixture is warmed to 80° C. for 6 h and then cooled to room temperature and stirred for another 16 h. Solvent is removed and the residue is partitioned between EtOAc and water. The organic layer is separated, dried and concentrated to afford crude compound which is purified by flash column chromatography using EtOAc in hexanes followed by trituration with acetonitrile to afford the title compound (5.5 g, 91%).

1. temperatureThe reaction mixture is warmed to 80° C. for 6 h
2. temperaturecooled to room temperature
3. stirringstirred for another 16 h
4. customSolvent is removed
5. customthe residue is partitioned between EtOAc and water
6. customThe organic layer is separated
7. customdried
8. concentrationconcentrated
9. customto afford crude compound which
10. customis purified by flash column chromatography