反应详情

A solution of 2-fluoro-4-(2-hydroxyethyl)benzonitrile (22.5 g, 136 mmol) and MsCl (23.3 g, 205 mmol) in 200 mL of dry DCM was added dropwise TEA (27.5 g, 273 mmol) at 0° C. The resulting mixture was stirred at room temperature overnight before concentrating to dryness. The residue was dissolved in 300 mL of EtOAc and washed with 1 N HCl and brine, dried over anhydrous Na2SO4 and concentrated to afford crude 2-(4-cyano-3-fluorophenyl)ethyl methanesulfonate. MS m/z 244 (M+1)+.

1. concentrationbefore concentrating to dryness
2. dissolutionThe residue was dissolved in 300 mL of EtOAc
3. washwashed with 1 N HCl and brine
4. dry with materialdried over anhydrous Na2SO4
5. concentrationconcentrated