反应详情

温度

0 °C

To a cold (0° C.) solution H2SO4 (2.68 g, 27.3 mmol) in CH3CN (91 mL) was added dropwise a solution of 2-(4-(trifluoromethyl)-phenyl)-2-propanol (1.86 g, 9.1 mmol) in CH3CN (9.1 mL). The resulting reaction mixture was stirred at 0° C. for 1 h then at rt for 23 h. The solvent was evaporated under vacuo and H2O was added (20 mL). The mixture was extracted with Et2O (2×50 mL) and the combined organic layers were washed with H2O (2×20 mL), an aqueous solution of NaOH (1N) (2×20 mL), dried over MgSO4, filtered and evaporated to give the title compound as white solid (2.00 g, 90%). 1H NMR (CDCl3, 300 MHz) δ 7.69 (d, J=8.3 Hz, 2H), 7.59 (d, J=8.3 Hz, 2H), 2.10 (s, 3H), 1.79 (s, 6H). HPLC (Condition A), Rt: 3.18 min (HPLC purity: 97.2%).

1. customThe resulting reaction mixture
2. waitat rt for 23 h
3. customThe solvent was evaporated under vacuo and H2O
4. additionwas added (20 mL)
5. extractionThe mixture was extracted with Et2O (2×50 mL)
6. washthe combined organic layers were washed with H2O (2×20 mL)
7. dry with materialan aqueous solution of NaOH (1N) (2×20 mL), dried over MgSO4
8. filtrationfiltered
9. customevaporated