反应详情

To a solution of 2-(2-fluoro-3-iodo-4-methoxy-phenyl)-[1,3] dioxolane (5.284 g, 16.30 mmol) in acetone (170 mL) was added HCl (1N, 170 mL) and the solution stirred at room temperature for 48 hrs. The solution was extracted with ethyl acetate and washed successively with water, brine, dried (MgSO4), filtered and evaporated. The residue was purified on silica gel (eluent: 10% ethyl acetate in hexane) to give 2.22 g of 2-Fluoro-3-iodo-4-methoxy benzaldehyde (38% for 2 steps). 1H NMR (300 MHz; CDCl3): 4.00 (s, 3 H), 6.74 (d, J=8.4 Hz, 1 H), 7.88 (t, J=8.1 Hz, 1 H), 10.21 (s, 1 H).

1. extractionThe solution was extracted with ethyl acetate
2. washwashed successively with water, brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified on silica gel (eluent: 10% ethyl acetate in hexane)