反应详情

温度

100 °C

To a solution of ethyl (6E)-6-[(dimethylamino)methylidene]-1-(2-hydroxyethyl)-7-oxo-4,5,6,7-tetrahydro-1H-indazole-3-carboxylate 15 g (49 mmol) in 50 ml of anhydrous DMF, 14.4 g (147 mmol) of anhydrous potassium acetate and 12.60 g (73.0 mmol) of methylisourea sulfate were added. The reaction was stirred at 100° C. for 16 hours. The mixture was diluted with ethyl acetate, washed with H2O, dried over Na2SO4, filtered and evaporated. The crude was purified by column (ethyl acetate:hexane 1:3) to give the title compound 1.2 g (10%). HRMS (ESI) calcd for C15H18N4O4 [M+H]+ 319.3278 found 319.3256.

1. washwashed with H2O
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customThe crude was purified by column (ethyl acetate:hexane 1:3)