反应详情

温度

120 °C

A mixture of 3-amino-2-methylacrolein (8.5 g., 0.1 mol.) and dimedone (14 g., 0.1 mol.) was treated with triethylamine (5 ml.) and ammonium acetate (0.1 g.) and heated in an oil bath at 120° C with stirring for 20 hours. The cooled reaction mixture was diluted with 2N HCl (50 ml.) and extracted with ethyl acetate (2 × 50 ml.) and the extracts discarded. The aqueous solution was adjusted to pH 10.0 with sodium carbonate and extracted with ethyl acetate (3 × 50 ml.). The combined extracts were dried (MgSO4 and the solvent removed to give a residual oil which was distilled to give the title compound as a colourless oil (7.8 g., 40%) b.p. 80°/0.2 mm Hg. (RT = 2 min. 2% OV17, T=150°).

1. customThe cooled reaction mixture
2. extractionextracted with ethyl acetate (2 × 50 ml.)
3. extractionextracted with ethyl acetate (3 × 50 ml.)
4. dry with materialThe combined extracts were dried (MgSO4
5. customthe solvent removed
6. customto give a residual oil which
7. distillationwas distilled