反应详情

A suspension of 4-(2-tert-butylphenyl)-N-(4-hydroxyphenyl)piperazine-1-carboxamide (Example 174, 0.290 g, 0.82 mmol), methyl bromoacetate (0.163 g, 1.07 mmol), and potassium carbonate (0.227 g, 1.64 mmol) in DMF (3 mL) was stirred at room temperature for 24 h. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with saturated NaHCO3 solution and brine, dried over MgSO4, and the solvent was evaporated under reduced pressure to give the crude product, which was purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:10 to 50:50) to provide methyl [4-({[4-(2-tert-butylphenyl)piperazin-1-yl]carbonyl}amino)phenoxy]acetate (0.260 g, 75%) as a white powder.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with saturated NaHCO3 solution and brine
3. dry with materialdried over MgSO4
4. customthe solvent was evaporated under reduced pressure
5. customto give the crude product, which
6. customwas purified by flash column chromatography (silica gel, n-hexane/ethyl acetate=90:10 to 50:50)