反应详情

A solution of 4-fluoro-2-(methyloxy)aniline (Heterocycles 1992, 34, 2301-2311) (5.6 g, 40 mmol) and triethylamine (6.9 ml, 50 mmol) in dichloromethane (200 ml) at 0° C. was treated with acetyl chloride (2.85 ml, 40 mmol). After stirring at room temperature for 1 hour the solution was washed with 2N hydrochloric acid. The organic phase was separated, washed with water and brine then dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was purified by chromatography on silica gel (1:5 to 1:2 ethyl acetate in dichloromethane) to afford the title compound. MS (ES+) m/e 184 [M+H]+.

1. washwas washed with 2N hydrochloric acid
2. customThe organic phase was separated
3. washwashed with water and brine
4. dry with materialthen dried over anhydrous magnesium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by chromatography on silica gel (1:5 to 1:2 ethyl acetate in dichloromethane)