反应详情

To ethyl 2-(4-chloro-3-(dibutylcarbamoyl)-5-methyl-1H-pyrazol-1-yl)-5-(naphthalen-2-ylsulfonylcarbamoyl)benzoate (1.39 g, 2.13 mmol) in THF (12.0 mL) and MeOH (4.0 mL) was added 0.5N aq. NaOH solution (21.3 mL, 10.7 mmol). The resulting reaction mixture was stirred at room temperature for 1.5 h. The mixture was then neutralized with 1N aq. HCl solution (pH=7) and extracted with EtOAc (3×). The combined organic extracts were dried over Na2SO4, filtered and concentrated in vacuo. The crude oil was triturated with CH2Cl2 (3×) to give the title compound (1.04 g, 78%) as a white solid. 1H NMR (DMSO-d6) δ 13.36 (br s, 1H), 8.71 (s, 1H), 8.43 (d, J=2.0 Hz, 1H), 8.26 (d, J=8.1 Hz, 1H), 8.17 (dd, J=8.4, 2.2 Hz, 2H), 8.07 (d, J=8.1 Hz, 1H), 7.99 (dd, J=8.7, 1.9 Hz, 1H), 7.78-7.64 (m, 3H), 3.38 (t, J=7.4 Hz, 2H), 3.29 (t, J=7.4 Hz, 2H), 2.10 (s, 3H), 1.58-1.38 (m, 4H), 1.36-1.22 (m, 2H), 1.13 (dq, J=14.8, 7.4 Hz, 2H), 0.90 (t, J=7.4 Hz, 3H), 0.74 (t, J=7.4 Hz, 3H); MS(ESI+) m/z 625.2 (M+H)+.

1. customThe resulting reaction mixture
2. extractionextracted with EtOAc (3×)
3. dry with materialThe combined organic extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude oil was triturated with CH2Cl2 (3×)