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), methylcellosolve (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-HC (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-HC (150 ml.)
6. dry with materialThe organic layer is dried over sodium sulfate
7. filtrationfiltered
8. customevaporated to dryness