反应详情

To a solution of N-{[1-(4-amino-cyclohexyl)-azetidin-3-ylcarbamoyl]-methyl}-3-trifluoromethyl-benzamide trifluoroacetic acid salt (as prepared in Example 35 Step B, 0.24 g, 0.4 mmol) in methanol (2 mL) was added DIEA (Aldrich, 0.21 mL, 1.2 mmol) and acetonylacetone (Aldrich, 0.06 mL, 0.5 mmol). The resulting mixture was stirred at rt overnight and the volatile organics were removed by evaporation. The residue was dissolved in water, extracted with EtOAc, dried over Na2SO4. Filtration and evaporation gave a crude product, which was purified by column chromatography (eluent: EtOAc) to give the cis isomer as a white solid.

1. customthe volatile organics were removed by evaporation
2. dissolutionThe residue was dissolved in water
3. extractionextracted with EtOAc
4. dry with materialdried over Na2SO4
5. filtrationFiltration and evaporation