反应详情

To a solution of 2-(tert-butyldimethylsilyloxy)-2-(5-(5-chloro-4-(5-cyclopropyl-1H-pyrazol-3-ylamino) pyrimidin-2-yl)thiophen-2-yl)acetic acid (60 mg, 0.12 mmol, 1.0 equiv.) in tetrahydrofuran (10 mL) was added Et3N.3HF (0.06 mL, 0.36 mmol, 3.0 equiv.). The reaction mixture was stirred at room temperature overnight. The mixture was diluted with ethyl acetate, washed (brine), dried (Na2SO4), filtered and concentrated to give a residue, the residue was purified by silica gel column chromatography (PE:EA=1:1) to afford 2-(5-(5-chloro-4-(5-cyclopropyl-1H-pyrazol-3-ylamino)pyrimidin-2-yl)thiophen-2-yl)-2-hydroxyacetic acid (Compound 219) (30 mg, 64.6%). LC-MS (m/z): 392.0 [M+H]+. 1H NMR (400 MHz, DMSO-d6): δ 0.75-0.76 (m, 2H), 0.97-0.99 (m, 2H), 1.92-1.96 (m, 1H), 5.31 (s, 1H), 6.45 (s, 1H), 7.13 (d, J=3.2 Hz, 1H), 7.67 (d, J=3.6 Hz, 1H), 8.39 (s, 1H), 9.30 (s, 1H), 12.59 (bs, 1H).

1. washwashed (brine)
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a residue
6. customthe residue was purified by silica gel column chromatography (PE:EA=1:1)