反应详情

温度

78 °C

To a solution of 40a, 4-Methyl-2-{4′-trifluoromethyl-5-[1-(3-trifluoromethyl-benzenesulfonyl)-piperidin-3-yl]-biphenyl-3-yl}-pentanoic acid ethyl ester (47.0 mg, 0.072 mmol) in EtOH (4.0 ml) was added 2M KOH (.36 ml, 0.72 mmol). The reaction was heated to 78° C. for 2 hours, cooled to room temperature, and concentrated in vacuo. Purification via Gilson HPLC, gave the product as a white lyophilate. (31.8 mg, 71% ) 1H NMR (300 MHz, MeOD) δ ppm 0.84 (d, J=6.41 Hz, 6 H) 1.36-1.47 (m, J=13.42, 6.97, 6.76, 6.76 Hz, 1 H) 1.50-1.64 (m, J=16.81, 7.11, 3.77, 3.58 Hz, 2 H) 1.76-1.91 (m, 3 H) 2.43 (t, J=10.93 Hz, 2 H) 2.78-2.89 (m, 1 H) 3.63 (t, J=7.72 Hz, 1 H) 3.69-3.78 (m, 2 H) 7.16 (s, 1 H) 7.38 (d, J=19.59 Hz, 2 H) 7.61-7.77 (m, 5 H) 7.88-7.99 (m, 3 H) Calcd for C31H31F6NO4S (M+H) 627.64, Found 628.0.

1. temperaturecooled to room temperature
2. concentrationconcentrated in vacuo
3. customPurification via Gilson HPLC
4. customgave the product as a white lyophilate