반응 #1076753

반응 방정식

octene

dimethylchlorosilane

→

octyldimethylchlorosilane

수율 88.0%

용매

toluene

반응 조건

후처리

1. 1
   기타equipped with a stirrer
2. 2
   workup.ADDITIONthermometer, addition funnel, and condenser
3. 3
   온도After the temperature had been raised
4. 4
   기타the heating mantle was removed
5. 5
   온도Heat generation
6. 6
   workup.ADDITIONthe dropwise addition
7. 7
   기타exceed 80° C
8. 8
   workup.ADDITIONAfter the completion of this addition
9. 9
   기타Gas chromatographic analysis of the resulting reaction solution

실험 절차

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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