反应详情

To a solution of 2,2,2-trifluoro-1-{4-[(6-fluoropyridin-2-yl)oxy]-3-methoxyphenyl}ethanol (0.22 mmol; 70 mg) under argon in dichloromethane (2 mL) at −78° C. was added dropwise DAST (0.22 mmol; 29 μl). The reaction mixture was let come back to rt for 2 h and quenched with brine (3 ml). The aqueous phase was collected, neutralized with sodium bicarbonate and extracted twice with chloroform. The organic phases were combined, dried over MgSO4, concentrated and purified by preparative TLC on silica gel (ethyl acetate/cyclohexane—30/70) to yield the title compound (25 mg; 0.08 mmol; 37%).

1. customquenched with brine (3 ml)
2. customThe aqueous phase was collected
3. extractionextracted twice with chloroform
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. custompurified by preparative TLC on silica gel (ethyl acetate/cyclohexane—30/70)