3,3,3-Trifluoropropyl-trimethoxysilane → Piperidine, 1-[dimethoxy(3,3,3-trifluoropropyl)silyl]-2-ethyl-

Temperatur

70 °C

Following the same general procedure described on Example 1, a flask was charged with one mol (218 gm) of 3,3,3-trifluoropropyltrimethoxysilane was added to one mol of 2-ethylpiperdinylmagnesium chloride, the salt having been prepared in situ by adding 2-ethylpiperidine (120 g, 1.05 mol) to isopropylmagnesium chloride (1 mol) in 500 ml of tetrahydrofuran. The reaction was mildly exothermic and the temperature rose to 45° C. at the end of the addition time of one hour. The reaction mixture was refluxed at the pot temperature of 70° C. for one hour and then cooled to room temperature. The 3,3,3-trifluoropropyl(2-ethylpiperidino)dimethoxysilane was filtered under nitrogen atmosphere from the magnesium methoxychloride. The filter cake was washed with ether (2×200 ml) to obtain the residual product. The solvent was removed by distillation to a pot temperature of 100° C. The residue was distilled under vacuum to yield 263 g of 3,3,3-trifluoropropyl(2-ethylpiperidino)dimethoxysilane as a colorless oil (purity>98%); bp 70° C./0.1 mm. The total yield was 88% of theoretical.

1. customthe salt having been prepared in situ
2. customrose to 45° C. at the end of the addition time of one hour
3. temperaturecooled to room temperature
4. filtrationThe 3,3,3-trifluoropropyl(2-ethylpiperidino)dimethoxysilane was filtered under nitrogen atmosphere from the magnesium methoxychloride
5. washThe filter cake was washed with ether (2×200 ml)
6. customto obtain the residual product
7. customThe solvent was removed by distillation to a pot temperature of 100° C
8. distillationThe residue was distilled under vacuum

ORD-Eintrag

ord-2a799657f9bc46a9bbdcd5af5672a57c

Quelldatensatz

uspto-grants-2000_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06114558