反应详情

HATU (0.915 g, 2.41 mmol) and DIPEA (0.701 ml, 4.01 mmol) were added sequentially to a solution of (R)-4-(phenylthio)-3-(4-sulfamoyl-2-(trifluoromethylsulfonyl)phenylamino) butanoic acid (INTERMEDIATE 8, 1.0 g, 2.01 mmol) and 1-(2-(tert-butyldiphenylsilyloxy)ethyl)piperazine (INTERMEDIATE 20, 0.894 g, 2.21 mmol) in DMA (2.0 ml). Additional DMA (1.7 ml) was added and the resulting mixture was stirred at room temperature for 2 hrs. The mixture was diluted with EtOAc and the organic layer was washed with H2O (2×), 1N NaHSO4 (aq.) and saturated aq. NaHCO3. The organic layer was dried (Na2SO4), and concentrated under reduced pressure to provide the title product (2.0 g, yield: quantitative), which was used in the preparation of INTERMEDIATE 22 without further purification.

1. washthe organic layer was washed with H2O (2×), 1N NaHSO4 (aq.) and saturated aq. NaHCO3
2. dry with materialThe organic layer was dried (Na2SO4)
3. concentrationconcentrated under reduced pressure