反应详情

Concentrated hydrochloric acid (367 ml) was added dropwise to a mixture of 1-(4-carboxyphenyl)-2-nitroprop-1-ene (61.17 g) and iron powder (61.17 g) in dioxan (500 ml) at reflux. The heating was continued for 1 hour at the end of addition. The solution was cooled, water added, the dioxan evaporated and the residue extracted with chloroform and dried (MgSO4). Removal of the solvent gave a solid which was recrystallised from ethyl acetate to give 26 g of the title compound. τ (d6DMSO) 7.83 (3H, s), 6.14 (2H, s), 2.69 (2H, d, J=9 Hz), 2.05 (2H, d, J=9 Hz).

1. temperatureat reflux
2. additionThe heating was continued for 1 hour at the end of addition
3. temperatureThe solution was cooled
4. customthe dioxan evaporated
5. extractionthe residue extracted with chloroform
6. dry with materialdried (MgSO4)
7. customRemoval of the solvent
8. customgave a solid which
9. customwas recrystallised from ethyl acetate