反应详情

温度

78 °C

To compound 44a, 4-Methyl-2-{5-[1-(4-pyrrol-1-yl-benzyl)-piperidin-3-yl]-4′-trifluoromethyl-biphenyl-3-yl}-pentanoic acid ethyl ester (56.2, 0.09 mmol) in EtOH (5 ml) was added 2M KOH (0.5 ml, 0.93 mmol). The reaction was heated to 78° C. for 1.5 hours, cooled to room temperature, and concentrated in vacuo. Purification via Gilson HPLC, salt exchange with 1N HCl (aqueous) gave the product as a white lyophilate, (32 mg, 56% ). 1H NMR (300 MHz, MeOD) δ ppm 0.89-0.97 (m, 6 H) 1.50 (dt, J=13.28, 6.74 Hz, 1 H) 1.67 (dt, J=13.47, 6.64 Hz, 1 H) 1.89-2.03 (m, 3 H) 2.05-2.15 (m, 2 H) 3.06-3.22 (m, 2 H) 3.52-3.63 (m, 2 H) 3.76 (t, J=7.72 Hz, 1 H) 4.39 (d, J=2.64 Hz, 2 H) 6.29-6.33 (m, 2 H) 7.23-7.26 (m, 2 H) 7.33 (s, 1 H) 7.54 (d, J=19.97 Hz, 2 H) 7.61 (s, 4 H) 7.78 (q, J=8.41 Hz, 4 H), Calcd for C35H37F3N2O2 (M+H) 574.68, Found 575.4.

1. temperaturecooled to room temperature
2. concentrationconcentrated in vacuo
3. customPurification via Gilson HPLC, salt exchange with 1N HCl (aqueous)
4. customgave the product as a white lyophilate, (32 mg, 56% )