反应详情

温度

55 °C

A mixture of 4-cyanoindole (5.0 g, 35.2 mmol), sodium hydrogen carbonate (8.9 g, 105.6 mmol) and hydroxylamine hydrochloride (4.9 g, 70.4 mmol) in ethanol (200 ml) was heated at 55° C. overnight. Sodium hydrogen carbonate (5.9 g, 70 mmol) and hydroxylamine hydrochloride (4.9 g, 70.4 mmol) was added. The mixture was heated for 4 days until only a small amount of starting material was present. The inorganics were filtered off, washing the solid well with ethanol and evaporated off the solvent. The residue was triturated with diethyl ether to give 5.8 g of off-white solid. δH (400 MHz, methanol-d4) 6.76-6.78 (1H, m), 7.12 (1H, t), 7.24 (1H, dd), 7.29-7.33 (1H, m) 7.46 (1H, dd).

1. temperatureThe mixture was heated for 4 days until only a small amount of starting material
2. filtrationThe inorganics were filtered off
3. washwashing the solid well with ethanol
4. customevaporated off the solvent
5. customThe residue was triturated with diethyl ether