反应详情

Dimethyl 2-[4-(1-tert-butoxycarbonylpiperidin-4-ylidenemethyl)-2-nitrophenyl]malonate (1.65 g; 3.7 mmol) was dissolved in ethanol (50 ml), tin powder (1.31 g; 11 g atom) was added followed by conc. hydrochloric acid (10 ml) and the mixture heated at reflux for 3 h before being left to stand at ambient temperature for 18 h. Evaporated to dryness under reduced pressure, water added to the residue and the insoluble material removed by filtration. The filtrate and washings were combined and evaporated to dryness under reduced pressure and this residue extracted with hot methanol. The insoluble materials were further extracted with hot ethanol, the extracts combined and evaporated to dryness under reduced pressure to give the title compound (680 mg; 81%) as a brown foam.

1. temperaturethe mixture heated
2. temperatureat reflux for 3 h
3. waitbefore being left
4. customEvaporated to dryness under reduced pressure, water
5. additionadded to the residue
6. customthe insoluble material removed by filtration
7. customevaporated to dryness under reduced pressure
8. extractionthis residue extracted with hot methanol
9. extractionThe insoluble materials were further extracted with hot ethanol
10. customevaporated to dryness under reduced pressure