反应详情

To a solution of tert-butyl 4-(3-methoxy-4-((4-(2-(2-methoxy-2-oxoethyl)phenethyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)phenyl)piperazine-1-carboxylate (I6) (0.360 g, 0.572 mmol) in tetrahydrofuran (17 mL), methanol (3 mL) and water (5 mL) was added lithium hydroxide (0.042 g, 1.77 mmol) and the resulting mixture was stirred at room temperature for 20 hours. The reaction volatiles were evaporated in vacuo and the resulting residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate. The aqueous phase was extracted with ethyl acetate (3×20 mL) and the combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate (20 mL), dried (magnesium sulfate), filtered, evaporated in vacuo and dried to give the title compound (I7) (0.356 g, 100%) as a yellow foam; 1H NMR (300 MHz, CDCl3) δ 1.48 (s, 9H), 2.96-3.06 (m, 8H) 3.56-3.62 (m, 6H), 3.77 (s, 3H), 6.47-6.51 (m, 2H), 7.00-7.11 (m, 2H), 8.00 (brs, 2H) and 8.43 (s, 1H). LCMS Method B: rt 9.00 min; m/z 616.4 [M+H]+.

1. customThe reaction volatiles
2. customwere evaporated in vacuo
3. additionthe resulting residue was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate
4. extractionThe aqueous phase was extracted with ethyl acetate (3×20 mL)
5. washthe combined organic extracts were washed with saturated aqueous sodium hydrogen carbonate (20 mL)
6. dry with materialdried (magnesium sulfate)
7. filtrationfiltered
8. customevaporated in vacuo
9. customdried