反应详情

To a solution of 2-methoxy-5-fluorobenzaldehyde (11.093 g, 1 eq, available from Aldrich Chemical Company) in methanol at −10° C. under nitrogen atmosphere is added NaBH4 (7.515 g, 2.7 equiv.) portionwise. The solution is allowed to warm to room temperature and after 30 minutes the reaction solvent is removed under reduced pressure and replaced with dichloromethane. This solution is poured onto ice water and further extracted with dichloromethane. The organic fractions are collected and dried (MgSO4) and the solvent removed under reduced pressure to give the title compound as an oil (9.794 g, 87%). MW 156.16; C8H9FO2; 1H NMR (CDCl3): 2.58 (m, 1H), 3.81 (s, 3H), 4.63 (d, 2H, 6.3 Hz), 6.78 (dd, 1H, 8.9 Hz and 4.3 Hz), 6.94 (td, 1H, 8.5 Hz and 3.1 Hz), 7.04 (dd, 1H, 8.7 Hz and 3.1 Hz).

1. customis removed under reduced pressure
2. additionThis solution is poured onto ice water
3. extractionfurther extracted with dichloromethane
4. customThe organic fractions are collected
5. dry with materialdried (MgSO4)
6. customthe solvent removed under reduced pressure