反应详情

温度

60 °C

Ethyl 3-(5-cyano-1H-indazol-1-yl)propanoate D47 (3.6 g, 14.80 mmol) was dissolved in ethanol (40 ml), hydroxylamine hydrochloride (2.057 g, 29.6 mmol) and sodium bicarbonate (6.22 g, 74.0 mmol) were added. The mixture was heated at 60° C. overnight. Cooled, filtered and the filtrate was evaporated, dissolved in EtOAc, washed with water (3×20 ml), dried over MgSO4 and evaporated again to give (1.75 g) of product. A further 0.290 g of white crystals were recovered from the rotary evaporater. MS (ES+): C13H16N4O3 requires 276; found (MH+) 277.

1. temperatureCooled
2. filtrationfiltered
3. customthe filtrate was evaporated
4. dissolutiondissolved in EtOAc
5. washwashed with water (3×20 ml)
6. dry with materialdried over MgSO4
7. customevaporated again