반응 #1797480
ord-959305eaeb8f423aaafc3de2f8b812a8
반응 방정식
potassium carbonate
CF3OCF═CF2
Hexafluorobutanol
CF3CFHCF2CH2OH
→
CF3CFHCF2CH2OCF2CFHOCF3
반응 조건
온도
45°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The resulting reaction mixture
- 2온도The reactor was cooled
- 3여과the contents of the reactor filtered
- 4기타to remove the potassium carbonate
- 5workup.ADDITIONThe resulting product-containing filtrate
- 6workup.DISTILLATIONwas distilled
실험 절차
Hexafluorobutanol, CF3CFHCF2CH2OH (65.3 g, 0.34 mol), prepared essentially as described above (Compound 2), was combined with potassium carbonate (9.9 g, 0.072 mol) and 133 g of acetonitrile in a 600 mL Parr reactor. The temperature of the reactor was raised to 45° C. and CF3OCF═CF2 (65.6 g, 0.39 mol) added as a gas over about two hours. The resulting reaction mixture was stirred for about 18 hours at 45° C. The reactor was cooled and the contents of the reactor filtered to remove the potassium carbonate. The resulting product-containing filtrate was distilled using a concentric tube column, with the product cut boiling at 115-119° C. The product structure was confirmed by GCMS.