反应详情

A solution of 108 g (0.55 mol) of ethyl diethylphosphonoacetate in 150 ml of dry 1,2-dimethoxyethane was slowly added dropwise, while stirring and cooling with ice to a suspension of 13.2 g (0.55 mol) of sodium hydride (26.4 g of 50% oil suspension) in 50 ml of dry 1,2-dimethoxyethane, whereupon the mixture foamed vigorously. After all the solution had been added the mixture was stirred for another 30 minutes. It was then combined with a suspension of 150 g (0.5 mol) of 4-amino-3,4',5-trichloro-benzophenone in 800 ml of dry 1,2-dimethoxyethane and heated for one hour at reflux temperature, whereby a clear solution was formed. The solution was evaporated to dryness in vacuo, and the residue was distributed between chloroform and water. The organic phase was dried and evaporated to dryness in vacuo. After mixing with 150 ml of ethanol, crystallization set in. The crystals were suction-filtered off and washed with ethanol and petroleum ether.

1. additionAfter all the solution had been added the mixture
2. stirringwas stirred for another 30 minutes
3. temperatureheated for one hour
4. temperatureat reflux temperature, whereby a clear solution
5. customwas formed
6. customThe solution was evaporated to dryness in vacuo
7. customThe organic phase was dried
8. customevaporated to dryness in vacuo
9. additionAfter mixing with 150 ml of ethanol, crystallization
10. filtrationThe crystals were suction-filtered off
11. washwashed with ethanol and petroleum ether