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Silicon tetrachloride → 3,7-Dimethyloctyl trichlorosilane

HRID 1504241
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HRID 1504241 반응식
[Cl:1][Si:2]([Cl:5])(Cl)[Cl:3].[CH3:6][CH:7]([CH2:12][CH2:13][CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:8][CH2:9][Mg]Br>O1CCCC1>[CH3:6][CH:7]([CH2:12][CH2:13][CH2:14][CH:15]([CH3:17])[CH3:16])[CH2:8][CH2:9][Si:2]([Cl:5])([Cl:3])[Cl:1]
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참가 물질

4

반응물 2

HCID 24816Silicon tetrachlorideHCID 178443368HCID 178443368, 화합물

생성물 1

HCID 1240151143,7-Dimethyloctyl trichlorosilane수율 81%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-10 °C

실험 절차

Tetrahydrofuran (100 ml) and tetrachlorosilane (17.0 g, 100 mmol) were placed in a 500 mL four-necked flask in a nitrogen atmosphere, and cooled to −10° C. 3,7-dimethyloctyl magnesium bromide (Sigma-Aldrich Co. LLC., 1.0 M, 100 ml) was added dropwise, and the mixture was agitated for 1 hour at 10° C. or less. The temperature was raised gradually to room temperature over the course of about 1 hour, and the mixture was left standing overnight. The precipitated salt was filtered out, the tetrahydrofuran was removed by concentration under reduced pressure, and the mixture was distilled under reduced pressure to obtain the target 3,7-dimethyloctyl trichlorosilane (99-102° C./0.3 Torr, 22.3 g, yield 81%).

후처리

  1. temperatureThe temperature was raised gradually to room temperature over the course of about 1 hour
  2. waitthe mixture was left
  3. waitstanding overnight
  4. filtrationThe precipitated salt was filtered out
  5. customthe tetrahydrofuran was removed by concentration under reduced pressure
  6. distillationthe mixture was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-441c85eb8e944551a7a488a1fe124ec7
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09212254B2

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