反应详情

A mixture of [4-(4-amino-phenyl)-piperazin-1-yl]-phenyl-acetic acid methyl ester (50 mg, 0.15 mmol), nicotinic acid (23 mg, 0.18 mmol), and HATU (70 mg, 0.18 mmol) in DMF (2 mL) was treated with iPr2NEt (32 μL, 0.18 mmol). After 16 h, the mixture was diluted with H2O and extracted with DCM. The organic layer was washed with satd. aq. NaHCO3 and brine, dried (MgSO4), and concentrated to give an oil, which was purified by PTLC to give a tan solid (51 mg, 77%). MS (ESI): mass calcd. for C25H26N4O3, 430.50; m/z found, 431.4 [M+H]+. 1H NMR (CDCl3): 9.07-9.06 (m, 1H), 8.77-8.76 (m, 1H), 8.20-8.18 (m, 1H), 8.01 (s, 1H), 7.68 (br s, 1H), 7.51-7.42 (m, 4H), 7.38-7.32 (m, 3H), 6.92-6.90 (m, 2H), 4.06 (s, 1H), 3.71 (s, 3H), 3.22-3.20 (m, 4H), 2.64-2.62 (m, 4H).

1. extractionextracted with DCM
2. washThe organic layer was washed with satd
3. dry with materialaq. NaHCO3 and brine, dried (MgSO4)
4. concentrationconcentrated
5. customto give an oil, which
6. customwas purified by PTLC