反应详情

温度

0 °C

Diazomethane (6.17 g, 147 mmol) was added dropwise to 3.02 g (21 mmol) of 3-butenal diethyl acetal in 10 ml of dry ether with intensive stirring at 0° C. Then 70 mg (0.312 mmol) of palladium (II) acetate in 50 ml of dry ether was added all at once. Then stirring at 0° C. continued until the evolution of N2 ceased (10 min.). The ether was distilled off to the reduced volume of the reaction mixture ca 10 ml. The precipitate was filtered off on a fritted glass funnel and the filtrate evaporated. The crude product (2.57 g) contained 97% of the title compound (GC) and was used without further purification.

1. stirringThen stirring at 0° C.
2. custom(10 min.)
3. distillationThe ether was distilled off to the reduced volume of the reaction mixture ca 10 ml
4. filtrationThe precipitate was filtered off on a fritted glass funnel
5. customthe filtrate evaporated
6. customwas used without further purification