反应详情

温度

90 °C

To a solution of 3,3-difluoro-3-(4-fluorophenyl)-propane-1-thiol (0.19 g, 0.92 mmol) in DMF (5 ml) in sealed tube are added 3-fluoro-N-(3-methyl-butyl)-pyridine-2-carboxylic acid amide (0.19 g, 0.92 mmol) and cesium carbonate (1.50 g, 4.60 mmol). The reaction mixture is heated at 90° C. for 2 h. After completion of the reaction, the reaction mixture is poured onto ice-water, extracted with EtOAc (3×30 ml). The combined organic layers are washed with brine (50 ml), water (30 ml), dried over sodium sulfate and evaporated to dryness to yield the crude product, which is purified by column chromatography (silica gel, 30% EtOAc/hexane) affording 3-[[3,3-Difluoro-3-(4-fluorophenyl)-propyl]sulfanyl]-N-(3-methyl-butyl)-pyridine-2-carboxylic acid amide (example 3) (0.15 g, 0.37 mmol, 41%). [M+H]+ 397.1.

1. customAfter completion of the reaction
2. additionthe reaction mixture is poured onto ice-water
3. extractionextracted with EtOAc (3×30 ml)
4. washThe combined organic layers are washed with brine (50 ml), water (30 ml)
5. dry with materialdried over sodium sulfate
6. customevaporated to dryness
7. customto yield the crude product, which
8. customis purified by column chromatography (silica gel, 30% EtOAc/hexane)