反应详情

Combine trifluoro-methanesulfonic acid 3,5-dichloro-4-[2-oxo-1-(2-trifluoromethanesulfonyl-4,5,6,7-tetrahydro-2H-indazol-5-yl)-pyrrolidin-3-ylmethyl]phenyl ester (Preparation 33) (0.5, 0.77 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-1H-pyrazole (0.484 g, 2.3 mmol), sodium carbonate (2.7 ml of 2.0 M, 5.4 mmol) in DME (12 mL) and degas with a stream of nitrogen. Add (Ph3P)4Pd (0.089 g, 0.07 mmol), and stir at 80° C. for 4 hour under nitrogen atmosphere. Cool to ambient temperature and add ethyl acetate (20 mL) and water (10 mL). Extract the aqueous phase with ethyl acetate (2×20 mL), dry (sodium sulfate) and condense under reduced pressure. Chromatography (silica, 95:5 CH2Cl2/MeOH) yields 0.144 g (42%) as a white solid MS (m/z): 445 (M+1).

1. extractionExtract the aqueous phase with ethyl acetate (2×20 mL)
2. customdry
3. custom(sodium sulfate) and condense under reduced pressure