反应详情

To 4-(trifluoromethyl)-1H-indole-5-carbonitrile (0.210 g, 0.85 mmol) in DMF (15 mL), was added NaOAc/3H2O (0.346 g, 2.54 mmol) and H2NOH/HCl (0.176 g, 2.54 mmol). The resulting mixture was stirred at rt for 15 h. H2O (30 mL) and sat'd aqueous NaHCO3 (45 mL) were added to the reaction mixture. Extraction with Et2O (3×50 mL) was followed by washing with brine, drying (Na2SO4), filtration, and concentration in vacuo. Trituration with hexanes/CH2Cl2 afforded 0.282 g of the title compound in good purity: 1NMR (400 MHz, CDCl3) δ 7.71 (d, J=8.6 Hz, 1H), 7.51 (d, J=8.6 Hz, 1H), 7.42 (d, J=3.4 Hz, 1H), 6.75 (m, 1H), 4.80 (s, 2H); MS (ESI): m/z 283 (M+1).

1. additionwere added to the reaction mixture
2. extractionExtraction with Et2O (3×50 mL)
3. washby washing with brine
4. customdrying
5. filtration(Na2SO4), filtration, and concentration in vacuo