3,3,3-Trifluoropropyl-trimethoxysilane → HCID 19900044、化合物

温度

0 °C

Under nitrogen, a 500 ml Schlenk flask was cooled to 0° C. and charged with 150 ml hexane and 3,3,3-trifluoropropyl trimethoxy silane (0.075 mol, 15 ml). A nitrogen purged addition funnel was fitted to the flask and charged with tert-butyllithium (0.075 mol, 34 ml). This was added dropwise to the cooled flask creating a cloudy, white precipitate (LiOCH3). After addition (1 hour), the addition funnel was washed with 20 ml of hexane. The ice bath was removed and the reaction mixture was allowed to warm to room temperature. The flask was fitted with a reflux condenser and the reaction mixture refluxed for two hours. After cooling to room temperature, the reaction mixture was filtered through a medium porosity filter tube, using Celite diatomaceous earth and glass wool as a filtering aid. A white solid was collected, which weighed 11.13 g wet (theoretical=3.0 grams of LiOCH3). The hexane was removed from the filtrate to give 20.33 g of a clear yellow oil.

1. customA nitrogen purged
2. additionaddition funnel
3. customwas fitted to the flask
4. additionThis was added dropwise to the cooled flask
5. additionAfter addition (1 hour)
6. washthe addition funnel was washed with 20 ml of hexane
7. customThe ice bath was removed
8. temperatureto warm to room temperature
9. customThe flask was fitted with a reflux condenser
10. temperaturethe reaction mixture refluxed for two hours
11. temperatureAfter cooling to room temperature
12. filtrationthe reaction mixture was filtered through a medium porosity
13. filtrationfilter tube
14. customA white solid was collected
15. customThe hexane was removed from the filtrate

ORDレコード

ord-bc68d895745540ba8582917d811e8f37

出典データセット

uspto-grants-1992_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05102842