反应详情

温度

0 °C

Catalyst 10% Pd/C(200 mg) was placed in a 3-necked round bottom flask and cooled at 0° C. Triisopropylsilane (3.32 g, 21 mmol) was added, followed by perflurooctanoyl chloride (7.9 g, 18.2 mmol). The mixture was allowed to warm to room temperature and was then controlled at 25°-27° C. during the exothermic reaction. After 3 hr, GC analysis showed aldehyde/acid chloride ratio=94/6. Another 0.26 mL of silane was added and stirring was continued for 1 hr. Vacuum transfer gave liquid which was chilled at -25° C. The resulting solid was shaken with petroleum ether, chilled at -25° C., and separated again. In this way, 6.48 g of product was obtained, mp ca. -5° C. NMR spectra were as described in Example 1.

1. temperatureto warm to room temperature
2. customwas then controlled at 25°-27° C. during the exothermic reaction
3. waitwas continued for 1 hr
4. customVacuum transfer gave liquid which
5. temperaturewas chilled at -25° C
6. temperaturechilled at -25° C.
7. customseparated again