反应详情

温度

-78 °C

To a solution of 6-bromo-naphthalene-2-carboxylic acid methoxy-methyl-amide (Step c, 6.3 g, 21.4 mmol) in THF (200 mL) at −78° C., DIBAL (1M in THF, 25.7 mL, 25.7 mmol) was added. The mixture was stirred at −78° C. for 10 min, warmed to RT and stirred for 2 h. The reaction was poured into 1N HCl and extracted with EtOAc 3×. The combined organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude was purified by silica gel column chromatography with (5-20% EtOAc/hexane) to give the titled compound as a white solid. MS (ESI, pos. ion) m/z: 236.0 (M+1).

1. temperaturewarmed to RT
2. stirringstirred for 2 h
3. extractionextracted with EtOAc 3×
4. washThe combined organic layer was washed with water and brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude was purified by silica gel column chromatography with (5-20% EtOAc/hexane)