反应详情

2-Methyl-2-({4-[2-({6-[4-(trifluoromethoxy)phenyl]pyridazin-3-yl}amino)ethyl]-1,3-thiazol-2-yl}thio)propionic acid tert-butyl ester (520 mg) obtained in Example 213-2 was dissolved in dichloromethane (2 mL), trifluoroacetic acid (2 mL) was added, and the mixture was stirred at room temperature for 12 hr. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added, and the mixture was washed with saturated aqueous sodium hydrogen carbonate solution (the objective compound was extracted in the ethyl acetate layer). The ethyl acetate layer was washed with aqueous 10% citric acid solution and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=1:1 to 0:1) to give the title compound (233 mg) as a white amorphous.

1. concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
2. additionwas added
3. washthe mixture was washed with saturated aqueous sodium hydrogen carbonate solution (the objective compound
4. extractionwas extracted in the ethyl acetate layer)
5. washThe ethyl acetate layer was washed with aqueous 10% citric acid solution and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. customthe residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=1:1 to 0:1)