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

Temperatur

50 °C

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 tool 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, 4H), 1.75-1.50 (m, 4H), 0.16 (s, 18H).

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

ORD-Eintrag

ord-cbdab4d5425b4503888ca51212da8afd

Quelldatensatz

uspto-grants-1995_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05457215