反应详情

温度

0 °C

At 0° C. and with cooling, 156.32 g (620 mmol) of tert-butyl diethylphosphonoacetate were added dropwise to a suspension of 23.71 g (593 mmol) of sodium hydride (60% in mineral oil) in 1.0 liters of THF. After the addition had ended, the mixture was stirred at 0° C. for 30 min and a solution of 100.0 g (539 mmol) of 4-chloro-3-nitrobenzaldehyde in 200 ml of THF was then added. The reaction mixture was heated at RT overnight, and water and ethyl acetate were then added. The organic phase was removed, dried with magnesium sulphate and concentrated under reduced pressure. The residue was recrystallized from isopropanol. Drying under high vacuum gave 144.0 g (94.2% of theory) of the target product.

1. additionAfter the addition
2. temperatureThe reaction mixture was heated at RT overnight
3. customThe organic phase was removed
4. dry with materialdried with magnesium sulphate
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from isopropanol
7. customDrying under high vacuum
8. customgave 144.0 g (94.2% of theory) of the target product