反应详情

温度

-78 °C

To a solution of 4-bromo-N-pivaloylaniline (1.56 g, 6 mmol) in dry THF (50 ml) at −78° C. was added t-BuLi (1.5 M in pentane, 13.3 ml, 20 mmol) and the yellow mixture was stirred for 1 h at −78° C. under N2. The reaction was quenched with B(OCH3)3 (1.7 ml, 15 mmol) and stirred for another 1 h at −78° C. The reaction mixture was then warmed to room temperature and hydrolysed with 0.5 M hydrochloric acid (50 ml) and extracted with EtOAc (3×80 ml), dried (Na2SO4) and concentrated to ca. 40 ml. n-Hexane (120 ml) was added slowly and the colorless crystalline product was filtered off and dried, yielding 1.26 g (95%).

1. stirringstirred for another 1 h at −78° C
2. extractionextracted with EtOAc (3×80 ml)
3. dry with materialdried (Na2SO4)
4. concentrationconcentrated to ca. 40 ml
5. additionn-Hexane (120 ml) was added slowly
6. filtrationthe colorless crystalline product was filtered off
7. customdried
8. customyielding 1.26 g (95%)