反应详情

温度

105 °C

4.99 g (30.0 mmol) 3,4-dimethoxybenzaldehyde (Aldrich, Milwaukee, Wis.), 15.0 g (194 mmol) ammonium acetate (Fluka), and 70 g (930 Mmol) nitroethane, 98% (Aldrich) were combined in a 100 ml round bottom flask equipped with magnetic stirrer and nitrogen inlet. The reaction mixture was heated to 105° C. for 90 minutes and the solvent was removed under vacuum to give a dark yellow liquid which was recrystallized from cold methyl alcohol three times to give yellow-orange needles in 50% yield. 1H NMR spectra is shown in FIG. 3.

1. customequipped with magnetic stirrer and nitrogen inlet
2. customthe solvent was removed under vacuum
3. customto give a dark yellow liquid which
4. customwas recrystallized from cold methyl alcohol three times
5. customto give yellow-orange needles in 50% yield