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Silicon tetrachloride → 3,7-Dimethyloctyl trichlorosilane

HRID 1772571
ノート
印刷プレビュー

反応式

HRID 1772571 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24816Silicon tetrachlorideHCID 178443368HCID 178443368、化合物

生成物 1

HCID 1240151143,7-Dimethyloctyl trichlorosilane収率 81%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-10 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-26eff2af4a8a4e5cb14170aedc2fc015
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09249257B2

反応ノート

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