反应详情

9.2 g sodium thread (0.4 mol) was added to 300 mL anhydrous ethyl alcohol with stirring at room temperature. After the Na was dissolved completely, 30 mL diethyl malonate (0.2 mol) and 20 g allyl urea (0.2 mol) were added and refluxed for 5 hours. After the completion of reaction, sucking filtration was performed when the reaction solution was still hot. The filter cake was dissolved in 150 mL anhydrous ethyl alcohol and HCl was used to adjust the pH to 2˜3. After sucking filtration, the filtrate was left to stand for crystallization. After sucking filtration again, washing with anhydrous ethyl alcohol and drying, a white solid (19.5 g) was obtained. Yield: 58%, MS: 169 (M+1).

1. temperaturerefluxed for 5 hours
2. customAfter the completion of reaction
3. filtrationfiltration
4. dissolutionThe filter cake was dissolved in 150 mL anhydrous ethyl alcohol
5. filtrationfiltration
6. waitthe filtrate was left
7. customto stand for crystallization
8. filtrationfiltration again
9. washwashing with anhydrous ethyl alcohol
10. customdrying