反应详情

(+)-1-(4-Cyanophenyl)-5-(3,6-dimethyl-2,4-dioxo-1-(3-trifluoromethylphenyl)-1,2,3,4-tetrahydropyrimidin-5-yl)-1H-pyrazole-4-sulfonamide (prepared in Example 209) (46 mg) was dissolved in acetonitrile (1 ml) and thereto were added benzoic acid (13 mg), 4-dimethylaminopyridine (21 mg) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (25 mg) and the resulting mixture was stirred for three hours at room temperature. To the reaction solution were added 1N hydrochloric acid (20 ml) and ethyl acetate (30 ml×2) such that the intended products were extracted into an organic layer. The organic layer was washed with 1N hydrochloric acid (20 ml) and saturated saline (30 ml) successively, dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol) to afford N-(1-(4-cyanophenyl)-5-(3,6-dimethyl-2,4-dioxo-1-(3-trifluoromethylphenyl)-1,2,3,4-tetrahydropyrimidin-5-yl)-1H-pyrazol-4-ylsulfonyl)benzamide (51 mg).

1. extractionwere extracted into an organic layer
2. washThe organic layer was washed with 1N hydrochloric acid (20 ml) and saturated saline (30 ml) successively
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol)