反应详情

The product of Example 385E (100 mg, 0.19 mmol), O-benzotriazol-1-yl-N,N,N′,N′-tetramethyluronium tetrafluoroborate [TBTU] (79 mg, 0.24 mmol) and the product of Example 442C (90 mg., 0.26 mmol) in DMSO (1.0 mL) were treated with N,N-diisopropylethylamine (100 μL, 0.57 mmol) dropwise at room temperature and stirred under N2 for 2 hours. The reaction was diluted with WATER (10 mL) with stirring. The resulting precipitate was extracted with ethyl acetate (50 mL). The organic layer was washed with WATER (3×), saturated aqueous NaHCO3, then brine, dried over MgSO4, and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate:chloroform=4:1) to give the title compound as a pale yellow amorphous solid (112 mg, 69%).

1. stirringwith stirring
2. extractionThe resulting precipitate was extracted with ethyl acetate (50 mL)
3. washThe organic layer was washed with WATER (3×), saturated aqueous NaHCO3
4. dry with materialbrine, dried over MgSO4
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography (ethyl acetate:chloroform=4:1)