反应详情

(4-{4-[6-(2-Methyl-6-trifluoromethyl-pyridin-3-ylamino)-pyridin-3-yl]-phenyl}-cyclohexyl)-acetic acid methyl ester (332 g, 0.69 mmol) was dissolved in THF/MeOH (3:1, 4 mL) and to it was added aqueous LiOH (4M, 1 mL). The mixture was stirred at room temperature for 18 hours, then the organic solvent was removed via rotary evaporation. The remaining crude was diluted with water and the pH was adjusted to 2 with 1 M HCl. The resulting precipitate was collected by filtration and dried under vacuum to obtain the title compound as a white solid: 1H NMR (400 MHz, DMSO-d6) δ ppm 0.95-1.04 (m, 2H) 1.44 (dd, J=12.51, 2.91 Hz, 2H) 1.67 (br. s., 1H) 1.74-1.87 (m, 6H) 2.47 (m, 1H) 2.60 (s, 3H) 7.25 (d, J=8.59 Hz, 1H) 7.30 (d, J=8.34 Hz, 2H) 7.56 (d, J=8.34 Hz, 2H) 7.66 (d, J=8.34 Hz, 1H) 7.97 (dd, J=8.72, 2.65 Hz, 1H) 8.48 (d, J=2.27 Hz, 1H) 8.67 (d, J=8.34 Hz, 1H) 8.80 (s, 1H); MS (M+H)+470.3.

1. customthe organic solvent was removed via rotary evaporation
2. additionThe remaining crude was diluted with water
3. filtrationThe resulting precipitate was collected by filtration
4. customdried under vacuum