反应详情

A solution of ethyl(4-{4-[5-(4-tert-butylphenyl)-4-methyl-4H-[1,2,4]-triazol-3-yl sulfanyl]-2-heptyloxybenzylamino}phenyl)acetate obtained in Example 1 (2.5 g, 4 mmol) of a 2M aqueous potassium carbonate solution (32 ml) in methanol (65 ml) is heated under reflux for 3 hours. The organic phase is acidified at room temperature with a 2N hydrochloric acid solution to pH 5. The desired product is extracted by addition of ethyl acetate. The organic phase is washed with water, dried with magnesium sulfate and concentrated using a rotary evaporator. The product is purified by chromatography on a silica column, eluted with a heptane/ethyl acetate 4:6 mixture. After evaporation of the solvents, 1.7 g (70%) of the expected compound are recovered in the form of a yellow amorphous solid.

1. temperatureunder reflux for 3 hours
2. extractionThe desired product is extracted by addition of ethyl acetate
3. washThe organic phase is washed with water
4. dry with materialdried with magnesium sulfate
5. concentrationconcentrated
6. customa rotary evaporator
7. customThe product is purified by chromatography on a silica column
8. washeluted with a heptane/ethyl acetate 4:6 mixture
9. customAfter evaporation of the solvents, 1.7 g (70%) of the expected compound
10. customare recovered in the form of a yellow amorphous solid