反应详情

To a solution of (4-oxo-3,4-dihydro-phthalazin-1-yl)-phosphonic acid dimethyl ester (3.85 g, 15.9 mmol) in THF (30 mL) was added 4-nitro-thiophene-2-carbaldehyde (25) (2.5 g, 15.9 mmol) under nitrogen. Triethylamine (2.2 mL 15.9 mmol) was added dropwise over 10 minutes and then stirred at room temperature for 4 hours. The yellow suspension was poured in water (80 mL), and the then filtered, the solid was washed with water (15 mL), hexane (10 mL) and then diethyl ether (10 mL) and then dried in vacuo to afford a 4.1 g of the desired products. Two peaks in LC-MS analysis, (4.1 g, 94%) and required no further purification; m/z (LC-MS, ESP), RT=4.71 mins (M+H) 274, & RT=4.84 mins (M+H) 274;

1. filtrationthe then filtered
2. washthe solid was washed with water (15 mL), hexane (10 mL)
3. dry with materialdiethyl ether (10 mL) and then dried in vacuo