反应详情

温度

80 °C

To a solution of NaOEt in EtOH (60 mL, 21 w %) were added diethyl 2-(ethoxymethylene)malonate (10.4 mL, 52.0 mmol) and hydrazine monohydrate (5.04 mL, 104 mmol) with cooling in an ice-water bath. The resulting mixture was then heated at 80° C. for 4 h. After cooling to rt, HCl (1 N, 180 mL) was added to the reaction mixture and then extracted with EtOAc three time. The combined organic layers were washed with brine and dried over Na2SO4. A solid obtained after evaporation was washed with ether and dried under high vacuum to afford the titled compound as an off-white solid (4.42 g), which was used without further purification.

1. temperaturewith cooling in an ice-water bath
2. temperatureAfter cooling to rt
3. extractionextracted with EtOAc three time
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. customA solid obtained
7. customafter evaporation
8. washwas washed with ether
9. customdried under high vacuum