反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The following were ingredients were introduced into a stirrer-equipped four-neck flask: 164.8 g (651.2 mmol) diphenyldichlorosilane and 300 mL tetrahydrofuran. The resultant mixture was stirred at room temperature while a mixture of 60 g (542.7 mmol) of 81.4% pure trimethylsilanol and 65.9 g (651.2 mmol) of triethylamine was added dropwise. Stirring at room temperature was continued for an additional hour following completion of the addition, at which time the salt formed as a by-product of the reaction was removed by filtration. The filtrate was then distilled under reduced pressure to yield 118.7 g of a fraction boiling at 136.5° C.-142° C. under of 2 mm Hg, equivalent to a 71.4% yield of trimethylsiloxydiphenylchlorosilane. Analysis of this product by gas chromatography (GLC), nuclear magnetic resonance (NMR), and infrared spectrochemical analysis (IR) confirmed it to be trimethylsiloxydiphenylchlorosilane with the following structural formula. ##STR6##
WORKUP
后处理
- additionwere introduced into a stirrer-equipped four-neck flask
- additionwas added dropwise
- waitwas continued for an additional hour
- additioncompletion of the addition
- customat which time the salt formed as a by-product of the reaction
- customwas removed by filtration
- distillationThe filtrate was then distilled under reduced pressure