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

HRID 1504250
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1504250
[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) as 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 distillation under reduced pressure was performed to obtain the target bis(3,7-dimethyloctyl)dichlorosilane (Compound G21) (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, and distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-471a5d64b41744149808fba945665f7c
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09212254B2

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