تفاعل #94893

معادلة التفاعل

4-nitrobenzophenone

sodium hydride

diethyl ethoxycarbonylmethylphosphonate

→

title compound

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

المذيبات

1,2-dimethoxyethane

1,2-dimethoxyethane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر