반응 #2451

반응 방정식

3-methyl-1-buten-3-ol

triethylsilane

→

1,1-dimethyl-3-(triethylsilyl)propyl alcohol

수율 81.1%

용매

n-butanol

반응 조건

후처리

1. 1
   기타Into a four-necked 500 mL-flask equipped with a stirring apparatus
2. 2
   workup.ADDITIONwere charged
3. 3
   workup.ADDITIONAfter the completion of the addition, they
4. 4
   온도were heated
5. 5
   workup.STIRRINGstirred for about 20 hours
6. 6
   기타Meanwhile, the proceeding of reaction
7. 7
   workup.ADDITIONwas added for the proceeding of the reaction
8. 8
   workup.DISTILLATIONThe reaction mixture was distilled under reduced pressure

실험 절차

Into a four-necked 500 mL-flask equipped with a stirring apparatus, a thermometer and a dropping funnel, 81.2 g (0.943 mole) of 3-methyl-1-buten-3-ol and 0.2 g of an n-butanol solution containing chloroplatinic acid at a concentration of 2 weight % were charged, and they were heated to 80° C. with stirring. From the dropping funnel, 109.6 g (0.943 mole) of triethylsilane was dropwise added into the four-necked flask. After the completion of the addition, they were heated and stirred for about 20 hours. Meanwhile, the proceeding of reaction was traced by gas chromatography analysis. At the stage when the proceeding of the reaction stopped, an additional mount of the above n-butanol solution containing chloroplatinic acid was added for the proceeding of the reaction. The reaction mixture was distilled under reduced pressure to obtain 154.9 g (0.765 mole) of 1,1-dimethyl-3-(triethylsilyl)propyl alcohol as a fraction at 105° C./14-16 torr.

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