反应详情

温度

100 °C

To a solution of ethyl (6E)-6-[(dimethylamino)methylidene]-2-methyl-7-oxo-4,5,6,7-tetrahydro-1H-indole-3-carboxylate 2 g (7.22 mmol) in 20 mL of anhydrous DMF, 1.41 g (14.4 mmol) of anhydrous potassium acetate and 4.0 g (14.4 mmol) of methylisothiourea sulfate were added. The reaction was stirred at 100° C. for 3 hours. The mixture was diluted with ethyl acetate, washed with H2O, dried over Na2SO4, filtered and evaporated. The crude was purified by silica gel chromagraphy (ethyl acetate: hexane 4:6) to give as major compound 0.8 g of ethyl 8-methyl-2-(methylsulfanyl)-6,9-dihydro-5H-pyrrolo[3,2-h]quinazoline-7-carboxylate (40%)

1. washwashed with H2O
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. customevaporated
5. customThe crude was purified by silica gel chromagraphy (ethyl acetate: hexane 4:6)