Chlorotrimethylsilane → 3,8-Dioxa-2,9-disiladecane, 2,2,9,9-tetramethyl-

HRID 1740329

Reaktionsgleichung

Reaktionsgleichung von HRID 1740329
[CH2:1]([OH:6])[CH2:2][CH2:3][CH2:4][OH:5].[CH3:7][Si:8](Cl)([CH3:10])[CH3:9]>C[Si](N[Si](C)(C)C)(C)C>[Si:8]([O:5][CH2:4][CH2:3][CH2:2][CH2:1][O:6][Si:8]([CH3:10])([CH3:9])[CH3:7])([CH3:10])([CH3:9])[CH3:7]

Komponenten

4

Edukt 2

HCID 6397ChlorotrimethylsilaneHCID 80641,4-Butanediol

Produkt 1

HCID 1403213,8-Dioxa-2,9-disiladecane, 2,2,9,9-tetramethyl-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13838HexamethyldisilazaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

1,4-Butanediol (54 g, 0.60 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.3 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 (120 mL, 0.66 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. (3 h), and 150° C. (1.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 127.8 g of colorless oil, bp 97-99° C./15 mm. 1H NMR (CDCl3): 3.75-3.50 (m, 4 H), 1.75-1.50 (m, 4 H), 0.16 (s, 18 H).

Aufarbeitung

  1. customan exothermic reaction
  2. temperatureHeating
  3. customwas continued at 100° C.
  4. custom(3 h), and 150° C. (1.5 h)
  5. distillationDistillation

Quellen und Nachweise

ORD-Eintrag
ord-156f5532406741a79fc99e6874df5d47
Quelldatensatz
uspto-grants-1999_10
Patentnummer
US05969074

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