反应详情

272 g of zinc dust in 270 ml of tert.-butanol are boiled with 24.9 ml of 1,2-dibromoethane until evolution of gas ceases. 55.5 g of CuBr and 66.9 g of LiBr in 200 ml of THF are then carefully added at 50° C. When the exothermic reaction has died down, 272 g of E-4-(carbo-tert.-butoxy)-4'-(4-carbo-tert.-butoxy-styryl)-tolan in 1.7 l of THF and 560 ml of tert.-butanol are added and the reaction mixture is heated under reflux for 4 days. The resulting reaction mixture is then evaporated to dryness, taken up in CH2Cl2 and filtered and the filtrate is washed with dilute HCl, dried and concentrated by evaporation.

1. customWhen the exothermic reaction
2. temperaturethe reaction mixture is heated
3. temperatureunder reflux for 4 days
4. customThe resulting reaction mixture
5. customis then evaporated to dryness
6. filtrationfiltered
7. washthe filtrate is washed with dilute HCl
8. customdried
9. concentrationconcentrated by evaporation