反应详情

温度

90 °C

K2CO3 (50.5 mg, 0.37 mmol) was added to a stirred solution of biphenyl-4-carboxylicacid (2-oxo-2-piperazin-1-yl-ethyl)-amide TFA salt (80 mg, 0.18 mmol) in DMF (3 mL). 2-Trifluoromethyl benzyl bromide (52.2 mg, 0.22 mmol) was then added, and the resulting mixture was heated to 90° C. overnight. The product was extracted with ethyl acetate and the ethyl acetate layer was washed with saturated brine solution, dried over sodium sulphate and concentrated to afford 48 mg (45.7% yield) of biphenyl-4-carboxylicacid {2-[4-(2-trifluoromethyl-benzyl)-piperazin-1-yl]-2-oxo-ethyl}-amide. LC-MS purity: 94.3%, 1H NMR: (CDCl3) δ 7.9 (d, 2H), 7.8-7.7 (d, 1H), 7.7-7.6 (m, 5H), 7.55 (m, 1H), 7.5 (m, 2H), 7.4 (m, 3H), 4.3 (d, 2H), 3.7 (s, 4H), 3.5 (t, 2H), 2.5 (q, 4H).

1. extractionThe product was extracted with ethyl acetate
2. washthe ethyl acetate layer was washed with saturated brine solution
3. dry with materialdried over sodium sulphate
4. concentrationconcentrated