反应详情

N-(2-ethylhexyl) cyanoacetamide (60.4 g., 0.30 mole), 4-methoxy-3-butene-2-one (60.0 g., 0.60 mole), methylcello-solve (250 ml.) and 1,4-diazobicyclo [2.2.2.] octane (6.0 g.) are heated at reflux for 4 hours. Additional 4-methoxy-3-butene-2-one (30 g.) is added and reflux is continued for another 2 hours. The solvent is removed in vacuo to give an oil. The oil is dissolved in methylene chloride and extracted first with 2N--HCl (150 ml.) and then with water (2 × 250 ml.). The organic layer is dried over sodium sulfate, filtered and evaporated to dryness to give a 90% yield of crude product which is characterized by nmr and ir analysis.

1. temperatureat reflux for 4 hours
2. temperaturereflux
3. customThe solvent is removed in vacuo
4. customto give an oil
5. extractionextracted first with 2N
6. dry with materialThe organic layer is dried over sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness