反应详情

温度

50 °C

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate (D47) (1 g, 4.11 mmol) was dissolved in ethanol (30 ml) and sodium bicarbonate (1.73 g, 20.88 mmol) and hydroxylamine hydrochloride (571 mg, 8.22 mmol) were added. The reaction was left at room temperature overnight and then heated to 50° C. for 4 hours then left to cool overnight. The reaction mixture was filtered and the residue washed with ethanol. The ethanolic filtrate was evaporated to dryness in vacuo and then triturated with ether to give the title compound (764 mg) as a white solid of approximately 90% purity. MS (ES): C13H16N4O3 requires 276; found (MH+) 277.

1. waitthen left
2. temperatureto cool overnight
3. filtrationThe reaction mixture was filtered
4. washthe residue washed with ethanol
5. customThe ethanolic filtrate was evaporated to dryness in vacuo
6. customtriturated with ether