反应详情

7.75 g (22 mmol) of 3-acetoxyacetamido-5-fluoro-2-hydroxy-benzoic acid-(2,2,2,-trifluoro-ethyl)amide (Example 37d) is dissolved in 50 ml of dry THF. 1.35 g (25 mmol) of sodium methylate is added, stirred for 15 minutes at room temperature, 4.27 g (25 mmol) of benzylbromide is added and refluxed for 1 hour. The reaction solution is then cooled to room temperature, NaBr is filtered off, the filtrate is concentrated by evaporation in a vacuum and the residue is chromatographed on silica gel 60 with ethyl acetate/hexane. 5.2 g=53.4% of the theoretical yield is obtained as an amorphous solid.

1. temperaturerefluxed for 1 hour
2. temperatureThe reaction solution is then cooled to room temperature
3. filtrationNaBr is filtered off
4. concentrationthe filtrate is concentrated by evaporation in a vacuum
5. customthe residue is chromatographed on silica gel 60 with ethyl acetate/hexane
6. custom5.2 g=53.4% of the theoretical yield
7. customis obtained as an amorphous solid