反应详情

p-Toluenesulfonic acid monohydrate (38 mg, 0.2 mmol) was added to a toluene (30 ml) solution of 4-amino-5-cyano-2-fluoro-6-methylbiphenyl-3-yl methoxyacetate (I-58) (214 mg, 0.68 mmol), followed by stirring for 3 hours and a half with heating under reflux. After cooling to room temperature, the reaction liquid was diluted with ethyl acetate, washed with saturated sodium bicarbonate water and saturated brine, then dried over anhydrous magnesium sulfate. After filtration and concentration under reduced pressure, the resulting residue was subjected to column chromatography, and the eluate with n-hexane:ethyl acetate (4:1) was concentrated under reduced pressure to obtain the entitled compound (160 mg, 79%) as a pale yellow solid.

1. temperaturea half with heating
2. temperatureunder reflux
3. customthe reaction liquid
4. washwashed with saturated sodium bicarbonate water and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationAfter filtration and concentration under reduced pressure
7. concentrationthe eluate with n-hexane:ethyl acetate (4:1) was concentrated under reduced pressure