反应详情

Trifluoromethanesulphonic anhydride (6.2 g) was added dropwise to an ice cooled, stirred solution of methyl 2-(2,2-dimethylpropionylamino)-6-hydroxybenzoate (Intermediate 40, 5.02 g) and pyridine (3.16 g) in DCM (70 mL) and the mixture was stirred for 1 hour. The resulting solution was washed with 2M hydrochloric acid, filtered through a phase separator and the filtrate was evaporated in vacuo. The residue was purified by chromatography on silica, eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-15% to give methyl 2-(2,2-dimethylpropionylamino)-6-trifluoromethanesulfonyloxybenzoate (7.09 g) as a colourless oil.

1. temperaturecooled
2. washThe resulting solution was washed with 2M hydrochloric acid
3. filtrationfiltered through a phase separator
4. customthe filtrate was evaporated in vacuo
5. customThe residue was purified by chromatography on silica
6. washeluting with a mixture of ethyl acetate and cyclohexane with a gradient of 0-15%