반응 #94893

반응 방정식

4-nitrobenzophenone

sodium hydride

diethyl ethoxycarbonylmethylphosphonate

→

title compound

Ethyl 3-Phenyl-3-(4-nitrophenyl)propenoate

용매

1,2-dimethoxyethane

1,2-dimethoxyethane

반응 조건

후처리

1. 1
   workup.WAITwas continued overnight
2. 2
   기타the solvent was removed by evaporation in vacuo
3. 3
   기타The residue was partitioned between ethyl acetate and water
4. 4
   기타The layers were separated
5. 5
   추출the water layer was extracted with fresh ethyl acetate
6. 6
   기타The combined ethyl acetate solutions were evaporated in vacuo

실험 절차

To a stirred suspension of sodium hydride, derived from 10.56 g. of a 50% suspension in mineral oil, in 400 ml. of 1,2-dimethoxyethane was added 51.6 g. of diethyl ethoxycarbonylmethylphosphonate, during 1 hour. When gas evolution ceased, a solution of 47.7 g. of 4-nitrobenzophenone in 400 ml. of 1,2-dimethoxyethane was added, dropwise, during 1.5 hours. Stirring was continued overnight and then the solvent was removed by evaporation in vacuo. The residue was partitioned between ethyl acetate and water. The layers were separated, and the water layer was extracted with fresh ethyl acetate. The combined ethyl acetate solutions were evaporated in vacuo to give the title compound as an oil, which slowly solidified.

출처