Water → 2-[2-(Heptafluoropropoxy)-tetrafluoroethyl]-ethyl alcohol

Temperatur

150 °C

A mixture of C3F7OCF2CF2CH2CH2I (300 g, 0.68 mol) and N-methyl-formamide (300 mL), was heated to 150° C. for 26 h. Then the reaction was cooled to 100° C., followed by the addition of water to separate the crude ester. Ethyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester, and the reaction was stirred at 70° C. for 15 minutes. Then ethyl formate and ethyl alcohol were distilled out to give a crude product. The crude product was dissolved in ether, washed with aqueous sodium sulfite, water, and brine in turn, then dried over magnesium sulfate. The product was then distilled to give 199 g of C3F7OCF2CF2CH2CH2OH in 85% yield. The boiling point was 71˜73° C. at 40 mm Hg (5333 Pa).

1. temperatureThen the reaction was cooled to 100° C.
2. customto separate the crude ester
3. additionEthyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester
4. distillationThen ethyl formate and ethyl alcohol were distilled out
5. customto give a crude product
6. washwashed with aqueous sodium sulfite, water, and brine in turn
7. dry with materialdried over magnesium sulfate
8. distillationThe product was then distilled

ORD-Eintrag

ord-7a2ed9e57dfd44c7a0acfd7e3acb2d72

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08129567B2