反应详情

To a solution of 1-(4-fluorobenzyl)piperazin-2-one (2.17 grams, 10.4 mmol) in 50 ml MeCN was added 1,1′-carbonyldiimidazole (2.03 g, 12.5 mmol) and dimethylaminopyridine (64 mg, 0.52 mmol). The solution was stirred at room temperature for 1 hour, concentrated under vacuum, and then dissolved in a mixture of CH2Cl2/CHCl3. The organic solution was washed with water three times, dried over anhydrous sodium sulfate, filtered, and concentrated under vacuum. The residue was triturated with diethyl ether, and filtered to provide the title product as a white solid. 1H NMR (400 MHz, CDCl3) δ 7.91 (s, 1H), 7.27 (t, J=6.9 Hz, 2H), 7.21 (t, J=1.4 Hz, 1H), 7.13 (s, 1H), 7.05 (t, J=8.6 Hz, 2H), 4.60 (s, 2H), 4.34 (s, 2H), 3.80 (t, J=5.4 Hz, 2H), 3.40 (t, J=5.4 Hz, 2H); ES MS (M+1)=303.

1. concentrationconcentrated under vacuum
2. dissolutiondissolved in a mixture of CH2Cl2/CHCl3
3. washThe organic solution was washed with water three times
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue was triturated with diethyl ether
8. filtrationfiltered