反应详情

温度

-15 °C

5 ml of boron fluoride etherate were added to 400 ml of methylene chloride and the mixture was cooled to -15° C. A solution of 132 g (2 moles) of freshly distilled cyclopentadiene and 256 g (1.8 moles) of 3-formylcrotyl acetate was added dropwise, whilst stirring, at a rate such that the reaction temperature did not rise above -10° C. The reaction was then allowed to continue for 2 hours at -10° C., whilst stirring. For working up, about 0.5 kg of ice was added, the mixture was neutralized with sodium bicarbonate solution, the aqueous phase was separated off and the methylene chloride was removed under reduced pressure (12 mm Hg/50° C.). The reaction product which remained was subjected to fractional distillation, giving 337 g of main fraction (yield: 90%).

1. customdid not rise above -10° C
2. stirringwhilst stirring
3. customthe aqueous phase was separated off
4. customthe methylene chloride was removed under reduced pressure (12 mm Hg/50° C.)
5. distillationThe reaction product which remained was subjected to fractional distillation
6. customgiving 337 g of main fraction (yield: 90%)