HRID610718
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Hydrosilation of phenylacetylene with bis(dichlorosilyl)trichlorosilylmethane in the presence of Pd(PPh3)4. Into the same apparatus as described in Example 1 were added 1.0 g of bis(dichlorosilyl)trichlorosilylmethane, 0.102 g of Pd(PPh3)4, and 25 ml of dried benzene to form a mixture. The mixture was brought to reflux temperature and 0.32 ml of phenylacetylene added over a 10 minute period. The mixture was stirred at reflux temperature for an additional 8 hours and then the solvent removed at atmospheric pressure. The residue was vacuum distilled at 67 Pa to yield a mixture comprising 0.348 g of 1,1,3,3-tetrachloro-2-trichlorosilyl-4-phenyl-1,3-disilacyclopent-4-ene (TCD-GC area 43.9%).
WORKUP
后处理
- customto form a mixture
- additionadded over a 10 minute period
- temperatureat reflux temperature for an additional 8 hours
- customthe solvent removed at atmospheric pressure
- distillationdistilled at 67 Pa