反应详情

温度

80 °C

The mixture of methyl 6-chloro-5-{4-[1-(hydroxymethyl)cyclobutyl]-3-methoxyphenyl}-1H-indole-3-carboxylate (220 mg, 0.55 mmol) in aqueous sodium hydroxide (10%, 3 mL) and methanol (5 mL) was stirred at 80° C. for 16 hours. The mixture was acidified by concentrated HCl to pH˜4 and extracted with dichloromethane. The organic phases were combined, dried over sodium sulfate, filtered, and concentrated in vacuo to give a residue, which was purified by reverse phase HPLC to give the title compound (25 mg, 12%) as a white solid. MS (AP+) 368.1 (M−H2O+H)+, 408.1 (M+Na)+. 1H NMR (500 MHz, CD3OD) δ 8.03 (s, 1H), 7.98 (s, 1H), 7.57 (s, 1H), 7.08 (d, 1H), 6.98 (d, 2H), 3.86 (s, 2H), 3.80 (s, 3H), 2.36 (m, 4H), 2.11 (m, 1H), 1.86 (m, 1H)

1. extractionextracted with dichloromethane
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customto give a residue, which
6. customwas purified by reverse phase HPLC