反应详情

温度

-40 °C

2-(5-Bromo-2-methylphenoxy)-5-(trifluoromethyl)pyridine (1 g, 0.003 mol) and triisopropylborate (0.8 mL, 0.003 mol) were dissolved in toluene (20 mL) and THF (5 mL) and cooled to −78° C. under a N2 atmosphere. n-BuLi (2.69 mL, 0.003 mol) was added while maintaining the reaction at −70° C. and then the reaction was stirred for 1 h at −40° C. Gradually the temperature was increased to −20-0° C. and then the reaction was quenched with 2N HCl. The reaction mixture was warmed to RT, concentrated and extracted with EtOAc. The organic extract was dried over Na2SO4 and concentrated under reduced pressure to give the title compound (1.13 g). m/z (296.4, 298.3, M− H−).

1. temperaturewhile maintaining
2. customthe reaction at −70° C.
3. temperatureGradually the temperature was increased to −20-0° C.
4. customthe reaction was quenched with 2N HCl
5. temperatureThe reaction mixture was warmed to RT
6. concentrationconcentrated
7. extractionextracted with EtOAc
8. extractionThe organic extract
9. dry with materialwas dried over Na2SO4
10. concentrationconcentrated under reduced pressure