反应详情

温度

25 °C

10.3 g of sodium hydride with 20% paraffin oil (0.343 mol) were suspended in 350 ml of tetrahydrofuran while stirring, and 75 g of diethylphosphonoacetic acid morpholide (0.0283 mol) were added dropwise to the suspension over a period of 20 minutes while cooling with ice (internal temperature 25° C.). The mixture was allowed to react for an hour during which a clear solution was formed. 70 g (0.244 mol) of 3,4-dimethoxy-4'-nitrobenzophenone were added to this solution all at once, and the mixture was refluxed for 2 hour while stirring. The solution was then evaporated in vacuo in a rotary evaporator at 60° C., and the residue was dissolved in methylene chloride/water. The organic phase was washed with water, dried over sodium sulfate and evaporated in vacuo at 60° C. The residue was triturated with 300 ml of hot methanol. 70.4 g of the title compound were obtained in the form of a faintly beige powder (73% of theory), m.p. 149°-163° C.

1. customto react for an hour during which a clear solution
2. customwas formed
3. temperaturewas refluxed for 2 hour
4. stirringwhile stirring
5. customThe solution was then evaporated in vacuo in a rotary evaporator at 60° C.
6. dissolutionthe residue was dissolved in methylene chloride/water
7. washThe organic phase was washed with water
8. dry with materialdried over sodium sulfate
9. customevaporated in vacuo at 60° C
10. customThe residue was triturated with 300 ml of hot methanol