反应详情

温度

23 °C

The compound, 1-(4-Fluorophenyl)-2-(pyridin-4-yl)ethanedione, the procedure of which may be found in U.S. Pat. No. 5,656,644, Example 13(b) whose disclosure is incorporated herein by reference in its entirety, (0.2 g, 0.87 mmol), and 1,2-diaminoethane (0.1 g, 1.67 mmol) were dissolved in methylene chloride (1 mL) and stirred under argon at 23° C. for about 12 hours. The solvent was removed in vacuo and the residue was chromatographed on silica gel eluted with 1-3% methanol in methylene chloride. Recrystallization from methylene chloride hexane gave the title compound as an yellow crystalline solid. ES (+) MS m/e=254 (MH+)

1. customThe solvent was removed in vacuo
2. customthe residue was chromatographed on silica gel
3. washeluted with 1-3% methanol in methylene chloride
4. customRecrystallization from methylene chloride hexane