反应详情

温度

180 °C

438 g (2.38 moles) of 2,5,7,7-tetramethyloctanal, 202 g (2.38 moles) of cyanoacetic acid, 350 ml of toluene, 350 ml of dimethylformamide and 28.5 g of ammonium acetate were heated under a water separator for 4 h, while stirring. Thereafter, the toluene was distilled off and the remaining residue was heated for 2 h at 180° C. The cooled residue was poured onto ice water and 10 extracted with diethyl ether. The organic phase was washed in succession with NaHCO: solution and water and then distilled. 450 g (yield: 91% of theory) of 4,7,9,9-tetramethyldec-3-enenitrile of boiling point 83°-88° C./-.3 mbar were obtained. The fragrance note was waxy, floral and fresh.

1. distillationThereafter, the toluene was distilled off
2. additionThe cooled residue was poured onto ice water and 10
3. extractionextracted with diethyl ether
4. washThe organic phase was washed in succession with NaHCO
5. distillationsolution and water and then distilled