Silane, tris(1-methylethyl)- → HCID 131719393, compound

Participants

Reaction Conditions

Reaction Steps

A 3-necked round bottom flask was charged with 10% Pd/C (400 mg) and cooled to 0° C. Triisopropylsilane (6.44 g, 40.7 mmol) was added, and CF3CH2OCF2CF2COCl (9.15 g, 34.9 mmol) was added dropwise. The mixture was warmed to room temperature, and the exotherm was then controlled by a room temperature water bath. The mixture was stirred an additional 22 hr over which time an additional 0.2 g of catalyst was added. The product was removed by vacuum transfer at 27 Pa. After isolation of the lower layer and washing several times with petroleum ether at -25° C., there was obtained 4.32 g of colorless liquid. 19F NMR (glyme-d10): -74.4 (t of t'2, J=8.2, 2.7), -87.35 (m, OCF2), -128.27 (apparent quartet, J=4 Hz, CF2CHO). GC/MS showed the major product with a fragment ion of m/z=209.0023. Calcd. for C5H3F6O2 (M-F): 209.0037.

Provenance & Evidence