反应详情

Trifluoromethanesulphonic anhydride (2.06 g) was added dropwise to a solution of 2-cyano-5-methoxyphenol (1.0 g) in dry pyridine (20 ml) at 0° C. under an atmosphere of argon. Volatile material was removed by evaporation and the residue was dissolved in ethyl acetate (30 ml). The solution was washed with water (60 ml) and saturated sodium chloride solution (30 ml) and dried (MgSO4). The solvent was removed by evaporation and the residue purified by flash chromatography, eluting with ethyl acetate/hexane (1:3 v/v), to give (2-cyano-5-methoxyphenyl)trifluoromethanesulphonate (1.53 g) as an oil; NMR (CDCl3): 3.9(s,3H), 6.95(d,1H), 7.0(d,1H), 7.7(d,1H).

1. customVolatile material was removed by evaporation
2. dissolutionthe residue was dissolved in ethyl acetate (30 ml)
3. washThe solution was washed with water (60 ml) and saturated sodium chloride solution (30 ml)
4. dry with materialdried (MgSO4)
5. customThe solvent was removed by evaporation
6. customthe residue purified by flash chromatography
7. washeluting with ethyl acetate/hexane (1:3 v/v)