反应详情

1 mole (170 g) of ethyl atropate, 210 g of crotonaldehyde, 150 g of anhydrous sodium acetate and 0.6 l of acetanhydride are heated to boiling for 6 h. while stirring. Subsequently the main amount of the liquid phase is distilled off under vacuum, and the residue is extracted with 1 liter of hot ligroin. The residue of the ligroin phase is distilled. The product -- although being pure according to gas chromatography -- distills in a wide boiling range: b.p.0,1 130°-165°C. Yield: 105 g. It crystallizes when allowed to stand. M.P. 72°-73°C (from petroleum ether).

1. distillationSubsequently the main amount of the liquid phase is distilled off under vacuum
2. extractionthe residue is extracted with 1 liter of hot ligroin
3. distillationThe residue of the ligroin phase is distilled
4. distillationdistills in a wide boiling range
5. customb.p.0,1 130°-165°C
6. customIt crystallizes when