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3,7-Dimethyloctyl trichlorosilane → Bis(3,7-dimethyloctyl)dichlorosilane

HRID 1504244
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1504244
[CH3:1][CH:2]([CH2:9][CH2:10][CH2:11][CH:12]([CH3:14])[CH3:13])[CH2:3][CH2:4][Si:5]([Cl:8])([Cl:7])Cl.[CH3:15][CH:16]([CH2:21][CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:17][CH2:18][Mg]Br>O1CCCC1>[CH3:15][CH:16]([CH2:21][CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:17][CH2:18][Si:5]([CH2:4][CH2:3][CH:2]([CH3:1])[CH2:9][CH2:10][CH2:11][CH:12]([CH3:13])[CH3:14])([Cl:7])[Cl:8]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 1240151143,7-Dimethyloctyl trichlorosilaneHCID 178443368HCID 178443368, Verbindung

Produkt 1

HCID 78062573Bis(3,7-dimethyloctyl)dichlorosilaneAusbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
-20 °C

Versuchsvorschrift

Tetrahydrofuran (50 mL) and 3,7-dimethyloctyl trichlorosilane (11.27 g, 40.9 mmol) were placed in a 200 mL four-necked flask in a nitrogen atmosphere, and cooled to −20° C. 3,7-dimethyloctyl magnesium bromide (Sigma-Aldrich Co. LLC., 1.0 M, 42.9 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 bis(3,7-dimethyloctyl)dichlorosilane (Compound E27) (150-152° C./0.6 Torr, 11.3 g, yield 73%).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-dd357e8c809342b790a434378dba2f62
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09212254B2

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