Chlorotrimethylsilane → 2,2,4,7,7-Pentamethyl-3,6-dioxa-2,7-disilaoctane

HRID 2210284

Reaktionsgleichung

Reaktionsgleichung von HRID 2210284
[CH:1]([OH:5])=[C:2]([OH:4])[CH3:3].[CH3:6][Si:7](Cl)([CH3:9])[CH3:8]>C[Si](N[Si](C)(C)C)(C)C>[Si:7]([O:4][CH:2]([CH2:1][O:5][Si:7]([CH3:9])([CH3:8])[CH3:6])[CH3:3])([CH3:9])([CH3:8])[CH3:6]

Komponenten

4

Edukt 2

HCID 6397ChlorotrimethylsilaneHCID 58537889Prop-1-ene-1,2-diol

Produkt 1

HCID 5194882,2,4,7,7-Pentamethyl-3,6-dioxa-2,7-disilaoctane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 13838HexamethyldisilazaneLösungsmittel3×

Versuchsvorschrift

1,2-Propenediol (58.8 g, 0.77 mol) was placed in a 500 mL 3-necked RB flask and treated with 0.2 mL trimethylsilyl chloride. A small volume of HMDS (ca. 10 mL) was added, and an exothermic reaction took place as the mixture became homogeneous. The remainder of the HMDS (170 mL) was added at a controlled rate (ca. 3-5 mL/min), maintaining the reaction temperature at ca. 50°-70° C. Heating was continued at 100° C. (1.5 h), 120° C. (1.0 h), and 140° C. (2.5 h). GC analysis (method 1) revealed excess HMDS and one product. Distillation provided 147 g of colorless oil, bp 70°-72° C./10 mm. 1H NMR (CDCl3): 3.83 (m; 1H), 3.50 and 3.38 (AB pattern with additional coupling, 2H), 1.15 (d, J=7 Hz, 3H), 0.15 (partially resolved singlets, 18H).

Aufarbeitung

  1. customan exothermic reaction
  2. temperaturemaintaining the reaction temperature at ca. 50°-70° C
  3. temperatureHeating
  4. customwas continued at 100° C.
  5. custom(1.5 h), 120° C. (1.0 h), and 140° C. (2.5 h)
  6. distillationDistillation

Quellen und Nachweise

ORD-Eintrag
ord-6e1d4116137d4b8b8e4abea4e51cb1bb
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05457215

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