تفاعل #64740

معادلة التفاعل

triethylsilane

perfluorooctanoyl chloride

triethylsilane

→

liquid

المردود 112.9%

C7F15CHO

المردود 112.9%

ظروف التفاعل

المعالجة

1. 1
   أخرىthe temperature below ca. 6°-8° C
2. 2
   workup.STIRRINGthe mixture was stirred for 1.5 hr
3. 3
   workup.WAITAfter 1.0 hr

الإجراء التجريبي

A sample of triethylsilane (4.24 g, 36.5 retool) was cooled to 0° C. and treated with 10% Pd/C(0.35 g). After the exotherm subsided, perfluorooctanoyl chloride (15.8 g, 36.5 mmol) was added dropwise, controlling the temperature below ca. 6°-8° C. The mixture was stirred for 1.0 hr at 0° C. Another 0.59 g triethylsilane was added, and the mixture was stirred for 1.5 hr. An additional 0.13 g of triethylsilane was added. After 1.0 hr, vacuum transfer gave 16.4 g of liquid which was cooled at -25° C. for several hours. The top liquid layer was removed from the solid to provide ca. 10.5 g of the titled product. 19F NMR: -81.3 (t of t's, J=9.8, 2.3), -121.8 (m), -122.3 (m), -123.0 (m), -123.7 (m), -125.4 (t of m's, with JFCCH =3 Hz), -126.5 (m).

المصدر