反应详情

A mixture of 3-amino-5,5-dimethylcyclohex-2-enone (27.8g., 0.2 mol.) and 2-methyl-3-ethoxyacrolein (22.8 g., 0.2 mol.), in an apparatus equipped for downward distillation, was heated in an oil bath at 120° until the theoretical quantity of distillate was collected (13 ml.) The cooled residue was diluted with 2N HCl (50 ml.), extracted with ethyl acetate (3 × 50 ml.) and the combined extracts discarded. The aqueous solution was adjusted to pH 9.0 with sodium carbonate and extracted with ethyl acetate (3 × 50 ml.). The combined extracts were dried (MgSO4) and the solvent removed in vacuo and the residual oil distilled to give the title compound as a colourless oil (23 g., 53%) b.p. 83°/0.2 mm Hg. (RT = 2 min., 2% OV17, T=150° C).

1. customin an apparatus equipped for downward distillation
2. temperaturewas heated in an oil bath at 120° until the theoretical quantity of distillate
3. customwas collected (13 ml.) The cooled residue
4. additionwas diluted with 2N HCl (50 ml.)
5. extractionextracted with ethyl acetate (3 × 50 ml.)
6. extractionextracted with ethyl acetate (3 × 50 ml.)
7. dry with materialThe combined extracts were dried (MgSO4)
8. customthe solvent removed in vacuo
9. distillationthe residual oil distilled