反应详情

To a solution of 4-[1-(2-aminopyrimidin-4-yl)-3-methylindazol-6-yl]-2-[1-(triphenylmethyl)imidazol-4-yl]but-3-yn-2-ol (45 mg, 0.07 mmol) in DCM (2 ml) was added trifluoroacetic acid (0.4 ml). The reaction was allowed to stand at RT for 0.5 hr and then concentrated in vacuo. DCM (5 mL) and saturated aqueous sodium bicarbonate (2 mL) were added and the organics extracted (4×5 mL DCM extractions). The combined extracts were dried (Na2SO4), filtered and concentrated in vacuo. The crude product was purified by flash chromatography (Isolute, 0-10% methanol gradient in DCM) to surrender the title compound as a pale brown solid: 1H NMR (250 MHz, MeOD) delta 1.92 (3H, s), 2.58 (3H, s), 7.28-7.14 (2H, m), 7.39 (1H, dd, J=8.2, 1.2 Hz), 7.82-7.64 (2H, m), 8.19 (1H, d, J=5.8 Hz), 8.98 (1H, s); LC-MS: m/z=+360.05 (M+H)+.

1. concentrationconcentrated in vacuo
2. additionDCM (5 mL) and saturated aqueous sodium bicarbonate (2 mL) were added
3. extractionthe organics extracted
4. extraction(4×5 mL DCM extractions)
5. dry with materialThe combined extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude product was purified by flash chromatography (Isolute, 0-10% methanol gradient in DCM)