反应详情

Sodium hydride (2.82 g, 0,117 mol) was dissolved in 30 ml of absolute ethanol at 0° C. Valeramidine hydrochloride (16.71 g, 0.123 mol) was added to this solution, and after 15 minutes the solution was filtered and the collected solid was washed with 20 ml of ethanol and 50 ml of benzene. The combined filtrates were diluted with 750 ml of benzene, 15 g (0.117 mol) of methyl 3-formylacrylate was added, and the mixture was refluxed for 18.5 h using a trap to remove water. The solvents were removed under vacuum and the residue slurried in ether. Evaporation of the ether solution gave the title compound as an oil.

1. filtrationafter 15 minutes the solution was filtered
2. washthe collected solid was washed with 20 ml of ethanol and 50 ml of benzene
3. additionwas added
4. temperaturethe mixture was refluxed for 18.5 h
5. customto remove water
6. customThe solvents were removed under vacuum
7. customEvaporation of the ether solution