反应详情

Sodium hydride (1 equi.) was added to the solution of 4-(2,3-difluorophenoxy)-butan-1-ol (22), (1 equi.) and 1-bromopentane (1 equi.) in DMF (1 mL/mmole) and the reaction mixture was stirred at room temperature for 12 h,. quenched with water, extracted with ethyl acetate:hexane (1:1), washed with brine, dried over MgSO4, and concentrated in vacuo. Purification by chromatography on silica gel (5% EtOAc/hexanes) and recrystallization from acetonitrile gave 1,2-difluoro-3-(4-pentyloxybutoxy)-benzene (24), as a white solid (84%).

1. customquenched with water
2. extractionextracted with ethyl acetate:hexane (1:1)
3. washwashed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customPurification by chromatography
7. customon silica gel (5% EtOAc/hexanes) and recrystallization from acetonitrile