反应详情

A solution (1 M) of methyl 5-[(E)-2-(4-chlorophenyl)vinyl]4-nitrothiophene-2-carboxylate in triethyl phosphite was heated to reflux for 20 h. After cooling down a part of the solvent was evaporated under high vacuum (2 mbar, water bath 60° C.) then the residue was purified by flash chromatography on silica gel (1:20 acetone/toluene). Fractions containing the title compound along with some phosphorous impurities were concentrated to give a residue that was triturated with AcOEt/petroleum ether (1:9) and filtered to afford the title compound (16%) as a solid.

1. temperatureto reflux for 20 h
2. temperatureAfter cooling down a part of the solvent
3. customwas evaporated under high vacuum (2 mbar, water bath 60° C.)
4. customthe residue was purified by flash chromatography on silica gel (1:20 acetone/toluene)
5. additionFractions containing the title compound along with some phosphorous impurities
6. concentrationwere concentrated
7. customto give a residue that
8. customwas triturated with AcOEt/petroleum ether (1:9)
9. filtrationfiltered