反应 #1076753

反应方程式

octene

dimethylchlorosilane

→

octyldimethylchlorosilane

收率 88.0%

溶剂

toluene

反应条件

后处理

1. 1
   其他equipped with a stirrer
2. 2
   workup.ADDITIONthermometer, addition funnel, and condenser
3. 3
   温度After the temperature had been raised
4. 4
   其他the heating mantle was removed
5. 5
   温度Heat generation
6. 6
   workup.ADDITIONthe dropwise addition
7. 7
   其他exceed 80° C
8. 8
   workup.ADDITIONAfter the completion of this addition
9. 9
   其他Gas chromatographic analysis of the resulting reaction solution

实验过程

123 g (1.1 mol) 1 -octene and 100 microliters of a 2% toluene solution of chloroplatinic acid were placed in a 500-mL four-neck flask equipped with a stirrer, thermometer, addition funnel, and condenser and were heated to 70° C. After the temperature had been raised, the heating mantle was removed and 94.5 g (1 mol) dimethylchlorosilane was added dropwise from the addition funnel. Heat generation was observed immediately, and the dropwise addition was carried out gradually so as to avoid having the temperature of the reaction solution exceed 80° C. After the completion of this addition, the reaction was continued for 30 minutes at 80° C. Gas chromatographic analysis of the resulting reaction solution gave 88% octyldimethylchlorosilane. The reaction solution was cooled to room temperature and 200 g toluene was introduced. The addition funnel was then replaced with a Teflon tube and ammonia was bubbled in until the pH of the reaction solution reached 10. The ammonium chloride product was removed by filtration, and the filtrate was then distillatively purified at 160° C./0.5 mmHg to obtain the following disilazane in a purity of 98 weight %.

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