反应详情

To 1-(4-Fluorobenzyl)piperazin-2-one (0.50 g, 2.40 mmol, Example 1, Step 4) dissolved in methylene chloride (75 mL) was added diisopropylethylaime (0.84 mL, 4.80 mmol) and cyanogen bromide (0.28 g, 2.64 mmol) and the resultant solution was stirred overnight at room temperature. The solvent was removed in vacuo and the residue was purified by flash chromatography on silica gel using a 0-5% MeOH/CHCl3 gradient. The pure fractions were concentrated to yield the title compound as a white solid. 1H NMR (400 MHz, d6 DMSO) δ 7.31 (m, 2H), 7.18 (m, 2H), 4.54 (s, 2H), 3.98 (s, 2H), 3.49 (m, 2H), and 3.33 (m, 2H); ES MS (M+1)=234.3.

1. customThe solvent was removed in vacuo
2. customthe residue was purified by flash chromatography on silica gel using a 0-5% MeOH/CHCl3 gradient
3. concentrationThe pure fractions were concentrated