反应详情

A solution of 4-Methoxy-1H-indole-2-carboxylic acid (930 mg, 4.86 mmol), amine 5 (1.63 g, 4.86 mmol) and DIEA (2.5 ml, 14.58 mmol) in 20 ml of DMF is treated with solid TBTU (1.56 g, 4.86 mmol). The mixture is stirred over night and then evaporated. The crude residue is dissolved in EtOAc and washed twice with sodium bicarbonate (10%). The aqueous layers are re-extracted with DCM, the combined organic layers are washed with brine and dried over sodium sulfate. The crude product is then purified by chromatography on silicagel using DCM (saturated with ammonia) and MeOH (from 0% to 2%).

1. customevaporated
2. dissolutionThe crude residue is dissolved in EtOAc
3. washwashed twice with sodium bicarbonate (10%)
4. extractionThe aqueous layers are re-extracted with DCM
5. washthe combined organic layers are washed with brine
6. dry with materialdried over sodium sulfate
7. customThe crude product is then purified by chromatography on silicagel