反应详情

To solution of dimethyl malonate (0.22 mL, 1.65 mmol) in benzene (15 mL) and acetic acid (3 drops) was added 1-(4-fluorophenyl)-1H-indazol-5-carboxaldehyde (330 mg, 1.38 mmol). The reaction mixture was heated at reflux overnight. The reaction was quenched with sat. KH2PO4 and extracted with EtOAc×3. The organic layers were dried over MgSO4, filtered, and concentrated. The residue was purified on SiO2 by MPLC using a 1:9 to 1:3 EtOAc/hexane gradient. Obtained 424 mg (87% yield) of dimethyl 2-((1-(4-fluorophenyl)-1H-indazol-5-yl)methylene)malonate. MS found: (M+H)+=355.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux overnight
3. customThe reaction was quenched with sat. KH2PO4
4. extractionextracted with EtOAc×3
5. dry with materialThe organic layers were dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified on SiO2 by MPLC