Chlorotrimethylsilane → 3,9-Dioxa-2,10-disilaundecane, 2,2,10,10-tetramethyl-

HRID 1740330Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1740330
[CH2:1]([OH:7])[CH2:2][CH2:3][CH2:4][CH2:5][OH:6].[CH3:8][Si:9](Cl)([CH3:11])[CH3:10]>C[Si](N[Si](C)(C)C)(C)C>[Si:9]([O:6][CH2:5][CH2:4][CH2:3][CH2:2][CH2:1][O:7][Si:9]([CH3:11])([CH3:10])[CH3:8])([CH3:11])([CH3:10])[CH3:8]

Komponenten

4

Edukt 2

HCID 6397ChlorotrimethylsilaneHCID 81051,5-Pentanediol

Produkt 1

HCID 1431753,9-Dioxa-2,10-disilaundecane, 2,2,10,10-tetramethyl-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13838HexamethyldisilazaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

1,5-Pentanediol (65 g, 0.62 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.4 mL trimethylsilyl chloride. A portion of HMDS (ca. 20 mL) was added, and an exothermic reaction took place as the mixture became homogeneous. The remainder of the HMDS (130 mL, 0.71 mol total) was added at a controlled rate (ca. 3-5 mL/min), maintaining the reaction temperature at ca. 50° C. Heating was continued at 100° C. (1 h), and 150° C. (2.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 139 g of colorless oil, bp 47-49° C./0.1 mm. 1H NMR (CDCl3): 3.60 (t, J=7 Hz, 4 H), 1.57 (m, 4 H), 1.40 (m, 2 H), 0.12 (s, 18 H), consistent with the assigned structure.

Aufarbeitung

  1. customan exothermic reaction
  2. temperatureHeating
  3. customwas continued at 100° C.
  4. custom(1 h), and 150° C. (2.5 h)
  5. distillationDistillation

Quellen und Nachweise

ORD-Eintrag
ord-f9217f0feeab4266b5d6288cc8660c60
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05969074

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